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Sample records for purge-and-trap capillary column

  1. A purge-and-trap capillary column gas chromatographic method for the measurement of halocarbons in water and air

    Energy Technology Data Exchange (ETDEWEB)

    Happell, J.D.; Wallace, D.W.R.; Wills, K.D.; Wilke, R.J.; Neill, C.C.

    1996-06-01

    This report describes an automated, accurate, precise and sensitive capillary column purge- and -trap method capable of quantifying CFC-12, CFC-11, CFC-113, CH{sub 3}CCL{sub 3}, and CCL{sub 4} during a single chromatographic analysis in either water or gas phase samples.

  2. Selective removal of water in purge and cold-trap capillary gas chromatographic analysis of volatile organic traces in aqueous samples

    NARCIS (Netherlands)

    Noij, T.H.M.; van Es, A.J.J.; Cramers, C.A.M.G.; Rijks, J.A.; Dooper, R.P.M.

    1987-01-01

    The design and features of an on-line purge and cold-trap pre-concentration device for rapid analysis of volatile organic compounds in aqueous samples are discussed. Excessive water is removed from the purge gas by a condenser or a water permeable membrane in order to avoid blocking of the capillary

  3. Determination of C6-C10 aromatic hydrocarbons in water by purge-and-trap capillary gas chromatography

    Science.gov (United States)

    Eganhouse, R.P.; Dorsey, T.F.; Phinney, C.S.; Westcott, A.M.

    1993-01-01

    A method is described for the determination of the C6-C10 aromatic hydrocarbons in water based on purge-and-trap capillary gas chromatography with flame ionization and mass spectrometric detection. Retention time data and 70 eV mass spectra were obtained for benzene and all 35 C7-C10 aromatic hydrocarbons. With optimized chromatographic conditions and mass spectrometric detection, benzene and 33 of the 35 alkylbenzenes can be identified and measured in a 45-min run. Use of a flame ionization detector permits the simultaneous determination of benzene and 26 alkylbenzenes.

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

    Science.gov (United States)

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

    2007-09-01

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

  5. Assembly for connecting the column ends of two capillary columns

    International Nuclear Information System (INIS)

    Kolb, B.; Auer, M.; Pospisil, P.

    1984-01-01

    In gas chromatography, the column ends of two capillary columns are inserted into a straight capillary from both sides forming annular gaps. The capillary is located in a tee out of which the capillary columns are sealingly guided, and to which carrier gas is supplied by means of a flushing flow conduit. A ''straight-forward operation'' having capillary columns connected in series and a ''flush-back operation'' are possible. The dead volume between the capillary columns can be kept small

  6. Development and characterization of a novel plug and play liquid chromatography-mass spectrometry (LC-MS) source that automates connections between the capillary trap, column, and emitter.

    Science.gov (United States)

    Bereman, Michael S; Hsieh, Edward J; Corso, Thomas N; Van Pelt, Colleen K; Maccoss, Michael J

    2013-06-01

    We report the development and characterization of a novel, vendor-neutral ultra-high pressure-compatible (~10,000 p.s.i.) LC-MS source. This device is the first to make automated connections with user-packed capillary traps, columns, and capillary emitters. The source uses plastic rectangular inserts (referred to here as cartridges) where individual components (i.e. trap, column, or emitter) can be exchanged independent of one another in a plug and play manner. Automated robotic connections are made between the three cartridges using linear translation powered by stepper motors to axially compress each cartridge by applying a well controlled constant compression force to each commercial LC fitting. The user has the versatility to tailor the separation (e.g. the length of the column, type of stationary phase, and mode of separation) to the experimental design of interest in a cost-effective manner. The source is described in detail, and several experiments are performed to evaluate the robustness of both the system and the exchange of the individual trap and emitter cartridges. The standard deviation in the retention time of four targeted peptides from a standard digest interlaced with a soluble Caenorhabditis elegans lysate ranged between 3.1 and 5.3 s over 3 days of analyses. Exchange of the emitter cartridge was found to have an insignificant effect on the abundance of various peptides. In addition, the trap cartridge can be replaced with minimal effects on retention time (<20 s).

  7. Speciation of organotin compounds in waters and marine sediments using purge-and-trap capillary gas chromatography with atomic emission detection

    International Nuclear Information System (INIS)

    Campillo, Natalia; Aguinaga, Nerea; Vin-tilde as, Pilar; Lopez-Garcia, Ignacio; Hernandez-Cordoba, Manuel

    2004-01-01

    A procedure for the simultaneous determination of six organotin compounds, including methyl-, butyl- and phenyltins, in waters and marine sediments is developed. The analytes were leached from the solid samples into an acetic acid:methanol mixture by using an ultrasonic probe. The organotins were derivatized with sodium tetraethylborate (NaBEt 4 ) in the aqueous phase, stripped by a flow of helium, pre-concentrated in a trap and thermally desorbed. This was followed by capillary gas chromatography with microwave-induced plasma atomic emission spectrometry as the detection system (GC-AED). Each chromatographic run took 22 min, including the purge time. Calibration curves were obtained by plotting peak area versus concentration and the correlation coefficients for linear calibration were at least 0.9991. Detection limits ranged from 11 to 50 ng Sn l -1 for tributyltin and tetramethyltin, respectively. The seawater samples analyzed contained variable concentrations of mono-, di- and tributyl- and monophenyltin, ranging from 0.05 to 0.48 μg Sn l -1 , depending on the compound. Some of the sediments analyzed contained concentrations of dibutyl- and tributyltin of between 6.0 and 13.0 ng Sn g -1 . Analysis of the certified reference material PACS-2, as well as of spiked water and sediment samples showed the accuracy of the method. The proposed method is selective and reproducible, and is considered suitable for monitoring organotin compounds in water and sediment samples

  8. Speciation of organotin compounds in waters and marine sediments using purge-and-trap capillary gas chromatography with atomic emission detection

    Energy Technology Data Exchange (ETDEWEB)

    Campillo, Natalia [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain); Aguinaga, Nerea [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain); Vin-tilde as, Pilar [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain); Lopez-Garcia, Ignacio [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain); Hernandez-Cordoba, Manuel [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia (Spain)]. E-mail: hcordoba@um.es

    2004-11-08

    A procedure for the simultaneous determination of six organotin compounds, including methyl-, butyl- and phenyltins, in waters and marine sediments is developed. The analytes were leached from the solid samples into an acetic acid:methanol mixture by using an ultrasonic probe. The organotins were derivatized with sodium tetraethylborate (NaBEt{sub 4}) in the aqueous phase, stripped by a flow of helium, pre-concentrated in a trap and thermally desorbed. This was followed by capillary gas chromatography with microwave-induced plasma atomic emission spectrometry as the detection system (GC-AED). Each chromatographic run took 22 min, including the purge time. Calibration curves were obtained by plotting peak area versus concentration and the correlation coefficients for linear calibration were at least 0.9991. Detection limits ranged from 11 to 50 ng Sn l{sup -1} for tributyltin and tetramethyltin, respectively. The seawater samples analyzed contained variable concentrations of mono-, di- and tributyl- and monophenyltin, ranging from 0.05 to 0.48 {mu}g Sn l{sup -1}, depending on the compound. Some of the sediments analyzed contained concentrations of dibutyl- and tributyltin of between 6.0 and 13.0 ng Sn g{sup -1}. Analysis of the certified reference material PACS-2, as well as of spiked water and sediment samples showed the accuracy of the method. The proposed method is selective and reproducible, and is considered suitable for monitoring organotin compounds in water and sediment samples.

  9. Analytical characterization and optimization in the determination of trihalomethanes on drinking water by purge and trap coupled to a gas chromatography

    International Nuclear Information System (INIS)

    Costa Junior, Nelson Vicente da

    2010-01-01

    This work shows an analytical methodology developed and optimized to determine trihalomethanes level THMs, in drinking water samples, using purge and trap coupled to gas chromatography (GC-PT). THMs are byproducts water chlorination, these compounds must have a maximum of 100 μg.L -1 under Brazilian law, due these compounds be suspected human carcinogens base on studies in laboratory animals. The technique of purge and trap efficiently extracts these compounds from water, and the gas chromatograph separates the THMs. The GC uses a light polarity column and electron capture detector. This detector is selective and more sensitive in the detection of these compounds. The methodology was validated in terms of: linearity, selectivity, accuracy, precision, quantification limit, detection limit and robustness. The detection limit was less than 0,5 μg.L -1 . The accuracy and precision were adequate for testing the trace compounds. The drinking water samples were collected in the city of Suzano-SP, which belongs to 'Alto do Tiete', in this region lay 'Tiete' river with predominant vegetation. The THMs compound found in drinking water at higher concentrations was chloroform where the spread of values found between 15,9 to 111,0 μg.L -1 in drinking water. (author)

  10. Evaluation of the Tekmar 3100 Purge and Trap Agilent GC/MSD system for VOC analysis

    Energy Technology Data Exchange (ETDEWEB)

    Li, K.; Fingas, M.F. [Environment Canada, Ottawa, ON (Canada). Emergencies Science and Technology Div

    2004-07-01

    This presentation described the Tekmar automated purge and trap (PAT) modular analyzer for detecting and quantifying volatile organic compounds (VOCs) in relatively clean water samples. A large percentage of emergency response work involves VOC analysis under various matrices such as water or soil. PAT analysis is an extraction method in which the VOCs from a liquid sample are purged by helium and concentrated on an internal trap, where the analytes are thermally desorbed into a gas chromatograph or a gas chromatograph/mass spectrometer (GS/MS). This high degree of concentration results in good detection limits. The performance of the Tekmar PAT 31000 concentrator with autosampler and GC/MS system was evaluated using a 1 ppb and 100 ppb standard of the Method 524 mixture for some selected VOC on the list. The study also examined the purging parameters such as time and temperature. It also examined a new way of introducing gaseous samples through the 3-way purge vessel valve on the concentrator. The objective was to determine if the versatility of the system could be extended by using the the same instrument configuration for air sampling. Preliminary results indicate that it is not yet practical to use the system for air sampling. 3 tabs., 4 figs.

  11. Thermally stable dexsil-400 glass capillary columns

    International Nuclear Information System (INIS)

    Maskarinec, M.P.; Olerich, G.

    1980-01-01

    The factors affecting efficiency, thermal stability, and reproducibility of Dexsil-400 glass capillary columns for gas chromatography in general, and for polycyclic aromatic hydrocarbons (PAHs) in particular were investigated. Columns were drawn from Kimble KG-6 (soda-lime) glass or Kimox (borosilicate) glass. All silylation was carried out at 200 0 C. Columns were coated according to the static method. Freshly prepared, degassed solutions of Dexsil-400 in pentane or methylene chloride were used. Thermal stability of the Dexsil 400 columns with respect to gas chromatography/mass spectrometry (GC/MS) were tested. Column-to-column variability is a function of each step in the fabrication of the columns. The degree of etching, extent of silylation, and stationary phase film thickness must be carefully controlled. The variability in two Dexsil-400 capillary column prepared by etching, silylation with solution of hexa methyl disilazone (HMDS), and static coating is shown and also indicates the excellent selectivity of Dexsil-400 for the separation of alkylated aromatic compounds. The wide temperature range of Dexsil-400 and the high efficiency of the capillary columns also allow the analysis of complex mixtures with minimal prefractionation. Direct injection of a coal liquefaction product is given. Analysis by GC/MS indicated the presence of parent PAHs, alkylated PAHs, nitrogen and sulfur heterocycles, and their alkylated derivatives. 4 figures

  12. Wall modified photonic crystal fibre capillaries as porous layer open tubular columns for in-capillary micro-extraction and capillary chromatography

    International Nuclear Information System (INIS)

    Kazarian, Artaches A.; Sanz Rodriguez, Estrella; Deverell, Jeremy A.; McCord, James; Muddiman, David C.; Paull, Brett

    2016-01-01

    Wall modified photonic crystal fibre capillary columns for in-capillary micro-extraction and liquid chromatographic separations is presented. Columns contained 126 internal parallel 4 μm channels, each containing a wall bonded porous monolithic type polystyrene-divinylbenzene layer in open tubular column format (PLOT). Modification longitudinal homogeneity was monitored using scanning contactless conductivity detection and scanning electron microscopy. The multichannel open tubular capillary column showed channel diameter and polymer layer consistency of 4.2 ± 0.1 μm and 0.26 ± 0.02 μm respectively, and modification of 100% of the parallel channels with the monolithic polymer. The modified multi-channel capillaries were applied to the in-capillary micro-extraction of water samples. 500 μL of water samples containing single μg L"−"1 levels of polyaromatic hydrocarbons were extracted at a flow rate of 10 μL min"−"1, and eluted in 50 μL of acetonitrile for analysis using HPLC with fluorescence detection. HPLC LODs were 0.08, 0.02 and 0.05 μg L"−"1 for acenaphthene, anthracene and pyrene, respectively, with extraction recoveries of between 77 and 103%. The modified capillaries were also investigated briefly for direct application to liquid chromatographic separations, with the retention and elution of a standard protein (cytochrome c) under isocratic conditions demonstrated, proving chromatographic potential of the new column format, with run-to-run retention time reproducibility of below 1%. - Highlights: • Novel PS-DVB modified photonic crystal fibres for in-capillary micro-extraction. • New method for micro-extraction of PAHs and HPLC-FL detection at sub-ppb levels. • Demonstration of PS-DVB modified photonic crystal fibres for capillary bioseparations.

  13. Wall modified photonic crystal fibre capillaries as porous layer open tubular columns for in-capillary micro-extraction and capillary chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Kazarian, Artaches A. [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia); W.M. Keck FT-ICR-MS Laboratory, Department of Chemistry, North Carolina State University, Raleigh, NC (United States); Sanz Rodriguez, Estrella; Deverell, Jeremy A. [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia); McCord, James; Muddiman, David C. [W.M. Keck FT-ICR-MS Laboratory, Department of Chemistry, North Carolina State University, Raleigh, NC (United States); Paull, Brett, E-mail: Brett.Paull@utas.edu.au [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia); ARC Centre of Excellence for Electromaterials Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart, Tasmania 7001 (Australia)

    2016-01-28

    Wall modified photonic crystal fibre capillary columns for in-capillary micro-extraction and liquid chromatographic separations is presented. Columns contained 126 internal parallel 4 μm channels, each containing a wall bonded porous monolithic type polystyrene-divinylbenzene layer in open tubular column format (PLOT). Modification longitudinal homogeneity was monitored using scanning contactless conductivity detection and scanning electron microscopy. The multichannel open tubular capillary column showed channel diameter and polymer layer consistency of 4.2 ± 0.1 μm and 0.26 ± 0.02 μm respectively, and modification of 100% of the parallel channels with the monolithic polymer. The modified multi-channel capillaries were applied to the in-capillary micro-extraction of water samples. 500 μL of water samples containing single μg L{sup −1} levels of polyaromatic hydrocarbons were extracted at a flow rate of 10 μL min{sup −1}, and eluted in 50 μL of acetonitrile for analysis using HPLC with fluorescence detection. HPLC LODs were 0.08, 0.02 and 0.05 μg L{sup −1} for acenaphthene, anthracene and pyrene, respectively, with extraction recoveries of between 77 and 103%. The modified capillaries were also investigated briefly for direct application to liquid chromatographic separations, with the retention and elution of a standard protein (cytochrome c) under isocratic conditions demonstrated, proving chromatographic potential of the new column format, with run-to-run retention time reproducibility of below 1%. - Highlights: • Novel PS-DVB modified photonic crystal fibres for in-capillary micro-extraction. • New method for micro-extraction of PAHs and HPLC-FL detection at sub-ppb levels. • Demonstration of PS-DVB modified photonic crystal fibres for capillary bioseparations.

  14. Development of a multiplexed interface for capillary electrophoresis-electrospray ion trap mass spectrometry.

    Science.gov (United States)

    Li, Fu-An; Wu, Ming-Chi; Her, Guor-Rong

    2006-08-01

    A four-channel multiplexed electrospray capillary electrophoresis interface has been developed. This new interface permits up to four capillary electrophoresis columns to be sampled sequentially by means of a stepper motor and a notched rotating plate assembly, which at any instant occludes all but a single sprayer. In this design, four sheath liquid electrospray probes are oriented in a circular array situated 90 degrees relative to one another. The rotating metal disk, which contains a one-quarter notch, is mounted to the stepper motor assembly and is located between the sprayers and the entrance aperture of an ion trap mass spectrometer. By using the data acquisition signal from the ion trap mass spectrometer, the scan event is synchronized with the rotation of the metal disk. With this device, four discrete sample streams can be simultaneously analyzed, resulting in a 4-fold increase in analytical throughput.

  15. Recent advances in the preparation and application of monolithic capillary columns in separation science

    Energy Technology Data Exchange (ETDEWEB)

    Hong, Tingting; Yang, Xi; Xu, Yujing [Department of Analytical Chemistry, China Pharmaceutical University, Nanjing, 210009 (China); Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, Nanjing, 210009 (China); Ji, Yibing, E-mail: jiyibing@msn.com [Department of Analytical Chemistry, China Pharmaceutical University, Nanjing, 210009 (China); Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, Nanjing, 210009 (China)

    2016-08-10

    Novel column technologies involving various materials and efficient reactions have been investigated for the fabrication of monolithic capillary columns in the field of analytical chemistry. In addition to the development of these miniaturized systems, a variety of microscale separation applications have achieved noteworthy results, providing a stepping stone for new types of chromatographic columns with improved efficiency and selectivity. Three novel strategies for the preparation of capillary monoliths, including ionic liquid-based approaches, nanoparticle-based approaches and “click chemistry”, are highlighted in this review. Furthermore, we present the employment of state-of-the-art capillary monolithic stationary phases for enantioseparation, solid-phase microextraction, mixed-mode separation and immobilized enzyme reactors. The review concludes with recommendations for future studies and improvements in this field of research. - Highlights: • Preparation of novel monolithic capillary columns have shown powerful potential in analytical chemistry field. • Various materials including ionic liquids and nanoparticles involved into capillary monolithic micro-devices are concluded. • Click chemistry strategy applied for preparing monolithic capillary columns is reviewed. • Recent strategies utilized in constructing different capillary monoliths for enantiomeric separation are summarized. • Advancement of capillary monoliths for complex samples analysis is comprehensively described.

  16. Recent advances in the preparation and application of monolithic capillary columns in separation science

    International Nuclear Information System (INIS)

    Hong, Tingting; Yang, Xi; Xu, Yujing; Ji, Yibing

    2016-01-01

    Novel column technologies involving various materials and efficient reactions have been investigated for the fabrication of monolithic capillary columns in the field of analytical chemistry. In addition to the development of these miniaturized systems, a variety of microscale separation applications have achieved noteworthy results, providing a stepping stone for new types of chromatographic columns with improved efficiency and selectivity. Three novel strategies for the preparation of capillary monoliths, including ionic liquid-based approaches, nanoparticle-based approaches and “click chemistry”, are highlighted in this review. Furthermore, we present the employment of state-of-the-art capillary monolithic stationary phases for enantioseparation, solid-phase microextraction, mixed-mode separation and immobilized enzyme reactors. The review concludes with recommendations for future studies and improvements in this field of research. - Highlights: • Preparation of novel monolithic capillary columns have shown powerful potential in analytical chemistry field. • Various materials including ionic liquids and nanoparticles involved into capillary monolithic micro-devices are concluded. • Click chemistry strategy applied for preparing monolithic capillary columns is reviewed. • Recent strategies utilized in constructing different capillary monoliths for enantiomeric separation are summarized. • Advancement of capillary monoliths for complex samples analysis is comprehensively described.

  17. Determination of cyclic volatile methylsiloxanes in biota with a purge and trap method.

    Science.gov (United States)

    Kierkegaard, Amelie; Adolfsson-Erici, Margaretha; McLachlan, Michael S

    2010-11-15

    The three cyclic volatile methylsiloxanes (cVMS), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), and dodecamethylcyclohexasiloxane (D6), are recently identified environmental contaminants. Methods for the trace analysis of these chemicals in environmental matrices are required. A purge and trap method to prepare highly purified sample extracts with a low risk of sample contamination is presented. Without prior homogenization, the sample is heated in water, and the cVMS are purged from the slurry and trapped on an Isolute ENV+ cartridge. They are subsequently eluted with n-hexane and analyzed with GC/MS. The method was tested for eight different matrices including ragworms, muscle tissue from lean and lipid-rich fish, cod liver, and seal blubber. Analyte recoveries were consistent within and between matrices, averaging 79%, 68%, and 56% for D4, D5, and D6, respectively. Good control of blank levels resulted in limits of quantification of 1.5, 0.6, and 0.6 ng/g wet weight. The repeatability was 12% (D5) and 15% (D6) at concentrations 9 and 2 times above the LOQ. The method was applied to analyze cVMS in fish from Swedish lakes, demonstrating that contamination in fish as a result of long-range atmospheric transport is low as compared to contamination from local sources.

  18. Capillary pressure - saturation relations for supercritical CO2 and brine: Implications for capillary/residual trapping in carbonate reservoirs during geologic carbon sequestration

    Science.gov (United States)

    Wang, S.; Tokunaga, T. K.

    2014-12-01

    In geologic carbon sequestration (GCS), data on capillary pressure (Pc) - saturation (Sw) relations are routinely needed to appraise reservoir processes. Capillarity and its hysteresis have been often experimentally studied in oil-water, gas-water and three phase gas-oil-water systems, but fewer works have been reported on scCO2-water under in-situ reservoir conditions. Here, Pc-Sw relations of supercritical (sc) CO2 displacing brine, and brine rewetting the porous medium to trap scCO2 were studied to understand CO2 transport and trapping behavior in carbonate reservoirs under representative reservoir conditions. High-quality drainage and imbibition (and associated capillary pressure hysteresis) curves were measured under elevated temperature and pressure (45 ºC, 8.5 and 12 MPa) for scCO2-brine as well as at room temperature and pressure (23 ºC, 0.1 MPa) for air-brine in unconsolidated limestone and dolomite sand columns using newly developed semi-automated multistep outflow-inflow porous plate apparatus. Drainage and imbibition curves for scCO2-brine deviated from the universal scaling curves for hydrophilic interactions (with greater deviation under higher pressure) and shifted to lower Pc than predicted based on interfacial tension (IFT) changes. Augmented scaling incorporating differences in IFT and contact angle improved the scaling results but the scaled curves still did not converge onto the universal curves. Equilibrium residual trapping of the nonwetting phase was determined at Pc =0 during imbibition. The capillary-trapped amounts of scCO2 were significantly larger than for air. It is concluded that the deviations from the universal capillary scaling curves are caused by scCO2-induced wettability alteration, given the fact that pore geometry remained constant and IFT is well constrained. In-situ wettability alteration by reactive scCO2 is of critical importance and must be accounted for to achieve reliable predictions of CO2 behavior in GCS reservoirs.

  19. Development and Calibration of an Oil Spill Behavior Model.

    Science.gov (United States)

    1982-09-01

    7675A purge-and-trap sampler. The GC column was a wide bore 50 meter long glass capillary column coated with SE-30 (WCOT from Alltech Associates, Inc...commonly used CGS unit of 1 dyne/cm is 10- 9 N/m or 1 milli-Newtons/meter (mN/m). An advantage of the technique is that there is no solid surface in

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

    Science.gov (United States)

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

    2017-06-01

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

  1. Quantification of prominent volatile compounds responsible for muskmelon and watermelon aroma by purge and trap extraction followed by gas chromatography-mass spectrometry determination.

    Science.gov (United States)

    Fredes, Alejandro; Sales, Carlos; Barreda, Mercedes; Valcárcel, Mercedes; Roselló, Salvador; Beltrán, Joaquim

    2016-01-01

    A dynamic headspace purge-and-trap (DHS-P&T) methodology for the determination and quantification of 61 volatile compounds responsible for muskmelon and watermelon aroma has been developed and validated. The methodology is based on the application of purge-and-trap extraction followed by gas chromatography coupled to (ion trap) mass spectrometry detection. For this purpose two different P&T sorbent cartridges have been evaluated. The influence of different extraction factors (sample weight, extraction time, and purge flow) on extraction efficiency has been studied and optimised using response surface methodology. Precision, expressed as repeatability, has been evaluated by analysing six replicates of real samples, showing relative standard deviations between 3% and 27%. Linearity has been studied in the range of 10-6130 ng mL(-1) depending on the compound response, showing coefficients of correlation between 0.995 and 0.999. Detection limits ranged between 0.1 and 274 ng g(-1). The methodology developed is well suited for analysis of large numbers of muskmelon and watermelon samples in plant breeding programs. Copyright © 2015 Elsevier Ltd. All rights reserved.

  2. Comparison of monolithic silica and polymethacrylate capillary columns for LC

    Czech Academy of Sciences Publication Activity Database

    Moravcová, D.; Jandera, P.; Urban, J.; Planeta, Josef

    2004-01-01

    Roč. 27, 10-11 (2004), s. 789-800 ISSN 1615-9306 R&D Projects: GA ČR(CZ) GA203/02/0023 Keywords : monolithic column s * capillary HPLC * column testing Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 1.927, year: 2004

  3. In situ preparation of multilayer coated capillary column with HKUST-1 for separation of neutral small organic molecules by open tubular capillary electrochromatography.

    Science.gov (United States)

    Xu, Yin-Yin; Lv, Wen-Juan; Ren, Cui-Ling; Niu, Xiao-Ying; Chen, Hong-Li; Chen, Xing-Guo

    2018-01-12

    The popularity of novel nanoparticles coated capillary column has aroused widespread attention of researchers. Metal organic frameworks (MOFs) with special structure and chemical properties have received great interest in separation sciences. This work presents the investigation of HKUST-1 (Hong Kong University of Science and Technology-1, called Cu 3 (BTC) 2 or MOF-199) nanoparticles as a new type of coating material for capillary electrochromatography. For the first time, three layers coating (3-LC), five layers coating (5-LC), ten layers coating (10-LC), fifteen layers coating (15-LC), twenty layers coating(20-LC) and twenty-five layers coating (25-LC) capillary columns coated with HKUST-1 nanoparticles were synthesized by covalent bond with in situ, layer-by-layer self-assembly approach. The results of scanning electron microscopy (SEM), X-ray diffraction (XRD) and plasma atomic emission spectrometry (ICP-AES) indicated that HKUST-1 was successfully grafted on the inner wall of the capillary. The separating performances of 3-LC, 5-LC, 10-LC, 15-LC, 20-LC and 25-LC open tubular (OT) capillary columns were studied with some neutral small organic molecules. The results indicated that the neutral small organic molecules were separated successfully with 10-LC, 15-LC and 20-LC OT capillary columns because of the size selectivity of lattice aperture and hydrophobicity of organic ligands. In addition, 10-LC and 15-LC OT capillary columns showed better performance for the separation of certain phenolic compounds. Furthermore, 10-LC, 15-LC and 20-LC OT capillary columns exhibited good intra-day repeatability with the relative standard deviations (RSDs; %) of migration time and peak areas lying in the range of 0.3-1.2% and 0.5-4.2%, respectively. For inter-day reproducibility, the RSDs of the three OT capillary columns were found to be lying in the range of 0.3-5.5% and 0.3-4.5% for migration time and peak area, respectively. The RSDs of retention times for column-to-column

  4. Trace analysis of halogenated hydrocarbons in gaseous samples by on-line enrichment in an adsorption trap, on-column cold-trapping and capillary gas chromatography. I.Method and instrumentation

    NARCIS (Netherlands)

    Noij, T.H.M.; Fabian, P.; Borchers, R.; Janssen, F.; Cramers, C.A.M.G.; Rijks, J.A.

    1987-01-01

    A method is described for the determination of halocarbons in gaseous samples down to the ppt level (1:1012, v/v), consisting of successive on-line sub-ambient enrichment on an adsorbent, on-column cryofocusing, capillary gas chromatography and electron-capture detection. The quantitative aspects of

  5. Open tubular capillary column for the separation of cytochrome C tryptic digest in capillary electrochromatography.

    Science.gov (United States)

    Ali, Faiz; Cheong, Won Jo

    2015-10-01

    A silica capillary of 50 μm internal diameter and 500 mm length (416 mm effective length) was chemically modified with 4-(trifluoromethoxy) phenyl isocyanate in the presence of dibutyl tin dichloride as catalyst. Sodium diethyl dithiocarbamate was reacted with the terminal halogen of the bound ligand to incorporate the initiator moiety, and in situ polymerization was performed using a monomer mixture of styrene, N-phenylacrylamide, and methacrylic acid. The resultant open tubular capillary column immobilized with the copolymer layer was used for the separation of tryptic digest of cytochrome C in capillary electrochromatography. The sample was well eluted and separated into many components. The elution patterns of tryptic digest of cytochrome C were studied with respect to pH and water content in the mobile phase. This preliminary study demonstrates that open tubular capillary electrochromatography columns with a modified copolymer layer composed of proper nonpolar and polar units fabricated by reversible addition-fragmentation transfer polymerization can be useful as separation media for proteomic analysis. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. A novel ionic liquid monolithic column and its separation properties in capillary electrochromatography

    International Nuclear Information System (INIS)

    Wang Yu; Deng Qiliang; Fang Guozhen; Pan Mingfei; Yu Yang; Wang Shuo

    2012-01-01

    Highlights: ► ILs as functional monomer for capillary monolithic column. ► Separation of alkylbenzenes, thiourea analogues, and amino acids. ► The column generate a stable reversed EOF from pH 2.0 to 12.0. ► The column efficiency of 147,000 plates m −1 was obtained for thiourea. - Abstract: A novel ionic liquid (IL) monolithic capillary column was successfully prepared by thermal free radical copolymerization of IL (1-vinyl-3-octylimidazolium chloride, ViOcIm + Cl − ) together with lauryl methacrylate (LMA) as the binary functional monomers and ethylene dimethacrylate (EDMA) as the cross-linker in binary porogen. The proportion of monomers, porogens and cross-linker in the polymerization mixture was optimized in detail. The resulting IL-monolithic column could not only generate a stable reversed electroosmotic flow (EOF) in a wide pH range (2.0–12.0), but also effectively eliminate the wall adsorption of the basic analytes. The obtained IL-monolithic columns were examined by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR). These results indicated that the IL-monolithic capillary column possessed good pore properties, mechanical stability and permeability. The column performance was also evaluated by separating different kinds of compounds, such as alkylbenzenes, thiourea and its analogues, and amino acids. The lowest plate height of ∼6.8 μm was obtained, which corresponded to column efficiency (theoretical plates, N) of ∼147,000 plates m −1 for thiourea. ILs, as a new type of functional monomer, present a promising option in the fabrication of the organic polymer-based monolithic columns in CEC.

  7. Measurement of residual solvents in a drug substance by a purge-and-trap method.

    Science.gov (United States)

    Lakatos, Miklós

    2008-08-05

    The purge-and-trap (P&T) gas extraction method combined with gas chromatography was studied for its suitability for quantitative residual solvents determination in a water-soluble active pharmaceutical ingredient (API). Some analytical method performance characteristics were investigated, namely, the repeatability, the accuracy and the detection limit of determination. The results show that the P&T technique is--as expected--more sensitive than the static headspace, thus it can be used for the determination of residual solvents pertaining to the ICH Class 1 group. It was found that it could be an alternative sample preparation method besides the static headspace (HS) method.

  8. Capillary electrochromatography of inorganic cations in open tubular columns with a controllable capacity multilayered stationary phase architecture.

    Science.gov (United States)

    Kubán, Pavel; Kubán, Petr; Kubán, Vlastimil; Hauser, Peter C; Bocek, Petr

    2008-05-09

    In this paper capillary electrochromatography of alkali and alkaline-earth metal cations in open tubular capillary columns is described. Capillary columns are prepared by coating fused silica capillaries of 75 microm I.D. with poly(butadiene-maleic acid) copolymer (PBMA) in multiple layers. Thermally initiated radical polymerization is used to crosslink the stationary phase. Capillary columns with different number of stationary phase layers can be prepared and allow for the adjustment of separation selectivity in the electrochromatographic mode. Fast and sensitive separations of common inorganic cations are achieved in less than 6 min in a 60 cm capillary column with on-column capacitively coupled contactless conductivity detector. Limits of detection (S/N=3) for the determination of alkali and alkaline-earth metal cations range from 0.3 to 2.5 microM and repeatability is better than 0.5, 4.5 and 6.1% for migration times, peak heights and peak areas, respectively.

  9. Influence of local capillary trapping on containment system effectiveness

    Energy Technology Data Exchange (ETDEWEB)

    Bryant, Steven [University Of Texas At Austin, Austin, TX (United States). Center for Petroleum and Geosystems Engineering

    2014-03-31

    Immobilization of CO2 injected into deep subsurface storage reservoirs is a critical component of risk assessment for geologic CO2 storage (GCS). Local capillary trapping (LCT) is a recently established mode of immobilization that arises when CO2 migrates due to buoyancy through heterogeneous storage reservoirs. This project sought to assess the amount and extent of LCT expected in storage formations under a range of injection conditions, and to confirm the persistence of LCT if the seal overlying the reservoir were to lose its integrity. Numerical simulation using commercial reservoir simulation software was conducted to assess the influence of injection. Laboratory experiments, modeling and numerical simulation were conducted to assess the effect of compromised seal integrity. Bench-scale (0.6 m by 0.6 m by 0.03 m) experiments with surrogate fluids provided the first empirical confirmation of the key concepts underlying LCT: accumulation of buoyant nonwetting phase at above residual saturations beneath capillary barriers in a variety of structures, which remains immobile under normal capillary pressure gradients. Immobilization of above-residual saturations is a critical distinction between LCT and the more familiar “residual saturation trapping.” To estimate the possible extent of LCT in a storage reservoir an algorithm was developed to identify all potential local traps, given the spatial distribution of capillary entry pressure in the reservoir. The algorithm assumes that the driving force for CO2 migration can be represented as a single value of “critical capillary entry pressure” Pc,entrycrit, such that cells with capillary entry pressure greater/less than Pc,entrycrit act as barriers/potential traps during CO2 migration. At intermediate values of Pc,entrycrit, the barrier regions become more laterally extensive in the reservoir

  10. Dopamine-imprinted monolithic column for capillary electrochromatography.

    Science.gov (United States)

    Aşır, Süleyman; Sarı, Duygu; Derazshamshir, Ali; Yılmaz, Fatma; Şarkaya, Koray; Denizli, Adil

    2017-11-01

    A dopamine-imprinted monolithic column was prepared and used in capillary electrochromatography as stationary phase for the first time. Dopamine was selectively separated from aqueous solution containing the competitor molecule norepinephrine, which is similar in size and shape to the template molecule. Morphology of the dopamine-imprinted column was observed by scanning electron microscopy. The influence of the organic solvent content of mobile phase, applied pressure and pH of the mobile phase on the recognition of dopamine by the imprinted monolithic column has been evaluated, and the imprinting effect in the dopamine-imprinted monolithic polymer was verified. Developed dopamine-imprinted monolithic column resulted in excellent separation of dopamine from structurally related competitor molecule, norepinephrine. Separation was achieved in a short period of 10 min, with the electrophoretic mobility of 5.81 × 10 -5  m 2 V -1 s -1 at pH 5.0 and 500 mbar pressure. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Flow rate dependent extra-column variance from injection in capillary liquid chromatography.

    Science.gov (United States)

    Aggarwal, Pankaj; Liu, Kun; Sharma, Sonika; Lawson, John S; Dennis Tolley, H; Lee, Milton L

    2015-02-06

    Efficiency and resolution in capillary liquid chromatography (LC) can be significantly affected by extra-column band broadening, especially for isocratic separations. This is particularly a concern in evaluating column bed structure using non-retained test compounds. The band broadening due to an injector supplied with a commercially available capillary LC system was characterized from experimental measurements. The extra-column variance from the injection valve was found to have an extra-column contribution independent of the injection volume, showing an exponential dependence on flow rate. The overall extra-column variance from the injection valve was found to vary from 34 to 23 nL. A new mathematical model was derived that explains this exponential contribution of extra-column variance on chromatographic performance. The chromatographic efficiency was compromised by ∼130% for a non-retained analyte because of injection valve dead volume. The measured chromatographic efficiency was greatly improved when a new nano-flow pumping system with integrated injection valve was used. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. A novel ionic liquid monolithic column and its separation properties in capillary electrochromatography.

    Science.gov (United States)

    Wang, Yu; Deng, Qi-Liang; Fang, Guo-Zhen; Pan, Ming-Fei; Yu, Yang; Wang, Shuo

    2012-01-27

    A novel ionic liquid (IL) monolithic capillary column was successfully prepared by thermal free radical copolymerization of IL (1-vinyl-3-octylimidazolium chloride, ViOcIm(+)Cl(-)) together with lauryl methacrylate (LMA) as the binary functional monomers and ethylene dimethacrylate (EDMA) as the cross-linker in binary porogen. The proportion of monomers, porogens and cross-linker in the polymerization mixture was optimized in detail. The resulting IL-monolithic column could not only generate a stable reversed electroosmotic flow (EOF) in a wide pH range (2.0-12.0), but also effectively eliminate the wall adsorption of the basic analytes. The obtained IL-monolithic columns were examined by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR). These results indicated that the IL-monolithic capillary column possessed good pore properties, mechanical stability and permeability. The column performance was also evaluated by separating different kinds of compounds, such as alkylbenzenes, thiourea and its analogues, and amino acids. The lowest plate height of ~6.8 μm was obtained, which corresponded to column efficiency (theoretical plates, N) of ~147,000 plates m(-1) for thiourea. ILs, as a new type of functional monomer, present a promising option in the fabrication of the organic polymer-based monolithic columns in CEC. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. Wettability impact on supercritical CO2 capillary trapping: Pore-scale visualization and quantification

    Science.gov (United States)

    Hu, Ran; Wan, Jiamin; Kim, Yongman; Tokunaga, Tetsu K.

    2017-08-01

    How the wettability of pore surfaces affects supercritical (sc) CO2 capillary trapping in geologic carbon sequestration (GCS) is not well understood, and available evidence appears inconsistent. Using a high-pressure micromodel-microscopy system with image analysis, we studied the impact of wettability on scCO2 capillary trapping during short-term brine flooding (80 s, 8-667 pore volumes). Experiments on brine displacing scCO2 were conducted at 8.5 MPa and 45°C in water-wet (static contact angle θ = 20° ± 8°) and intermediate-wet (θ = 94° ± 13°) homogeneous micromodels under four different flow rates (capillary number Ca ranging from 9 × 10-6 to 8 × 10-4) with a total of eight conditions (four replicates for each). Brine invasion processes were recorded and statistical analysis was performed for over 2000 images of scCO2 saturations, and scCO2 cluster characteristics. The trapped scCO2 saturation under intermediate-wet conditions is 15% higher than under water-wet conditions under the slowest flow rate (Ca ˜ 9 × 10-6). Based on the visualization and scCO2 cluster analysis, we show that the scCO2 trapping process in our micromodels is governed by bypass trapping that is enhanced by the larger contact angle. Smaller contact angles enhance cooperative pore filling and widen brine fingers (or channels), leading to smaller volumes of scCO2 being bypassed. Increased flow rates suppress this wettability effect.

  14. Validity of using modified capillary column with larger diameter to study the Cs diffusion in local Taiwan laterite

    International Nuclear Information System (INIS)

    Tsing-Hai Wang; National Tsing Hua University, Hsinchu, Taiwan; Wen-Chun Yeh; Shih-Chin Tsai; Yi-Lin Jan; Shi-Ping Teng

    2008-01-01

    We have examined the working diameter of capillary columns with diameter of 5, 7, 10 and 20 mm. These modified capillary columns were carefully filled with local Taiwan laterite (LTL). The porosity and density of these packed columns was 0.51±0.02 g/g and 1.27±0.05 g/cm 3 , respectively. The diffusion experiments were then carried out in synthetic groundwater with Cs loading of 0.1mM at room temperature. Experimental results have shown that the diffusion profiles of modified capillary columns fit Fick's second law very well. This result revealed that the working diameter of a capillary column can be expanded to at least to 20 mm without affecting the validity of the derived diffusion coefficients. Among these columns, the ones with 5 mm diameter show the most consistent results of the derived K d , apparent and effective diffusion coefficients. Although the derived distribution and effective diffusion coefficients slightly decrease as the diameter of these columns increases due to the increase of the solid/liquid ratio. These values are still informative of the Cs diffusion in local Taiwan laterite. Moreover, our results clearly demonstrate the potential of using 'modified capillary method' to study the diffusion behaviors of concerned radionuclide because columns with large diameter enable the filling with more versatile geological substances. (author)

  15. New Liquid Phases for the Gas Chromatographic Separation of Strong Bases on Capillary Columns

    OpenAIRE

    Grob, K.

    2017-01-01

    The current practice of pretreating the solid support with free alkali to increase separation efficiency for basic compounds proved to be unsuitable for capillary columns. Instead of this, homogenous organic materials of high base strength are required. We found polyethylene imine (PEI) and polypropylene imine (PPI) to be very efficient as liquid phases of capillary columns for the separation of bases. The preparation of polymers is mentioned. Silanization or acetylation of the free hydroxyl ...

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

    Science.gov (United States)

    Hayes, J D; Malik, A

    2001-03-01

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

  17. Characterization of polymer-based monolithic capillary columns by inverse size-exclusion chromatography and mercury-intrusion porosimetry

    NARCIS (Netherlands)

    Urban, J.; Eeltink, S.; Jandera, P.; Schoenmakers, P.J.

    2008-01-01

    Organic-polymer monolithic capillary columns were prepared in fused-silica capillaries by a radical copolymerization reaction of butyl methacrylate and ethylene dimethacrylate monomers in the presence of 1,4-butanediol and 1-propanol as porogen solvents and azobisisobutyronitrile as the initiator.

  18. SEPARATION OF OCTYLPHENOL POLYETHER ALCOHOLS SURFACTANTS BY CAPILLARY COLUMN SFC AND HPLC

    Science.gov (United States)

    Separation of nonionic octylphenol polyether alcohols (OPA) by supercritical fluid chromatography (SFC) and HPLC is described. Using a density programming and a 50-μm i.d. capillary column, a total of 18 group oligomers was separated. The effects of the operating parameters, such...

  19. Comparison of two validated gas-chromatographic methods for the determination of trihalomethanes in drinking water Comparação de dois métodos cromatográficos validados para a dosagem de trialometanos em água potável

    OpenAIRE

    Maria Yumiko Tominaga; Antonio Flavio Mídio

    2003-01-01

    In this paper the results obtained using two validated gas-chromatographic procedures on drinking water for the determination of trihalomethanes are compared. The volatile compounds, chloroform (CF), bromodichloromethane (BDCM), dibromochloromethane (DBCM) and bromoform (BF) were detected by purge and trap capillary column gas-chromatography with electrolytic conductivity detector ( ELCD) and the simple and rapid gas-chromatographic method by electron capture detector (ECD) after liquid-liqui...

  20. Implementation of a fully automated process purge-and-trap gas chromatograph at an environmental remediation site

    International Nuclear Information System (INIS)

    Blair, D.S.; Morrison, D.J.

    1997-01-01

    The AQUASCAN, a commercially available, fully automated purge-and-trap gas chromatograph from Sentex Systems Inc., was implemented and evaluated as an in-field, automated monitoring system of contaminated groundwater at an active DOE remediation site in Pinellas, FL. Though the AQUASCAN is designed as a stand alone process analytical unit, implementation at this site required additional hardware. The hardware included a sample dilution system and a method for delivering standard solution to the gas chromatograph for automated calibration. As a result of the evaluation the system was determined to be a reliable and accurate instrument. The AQUASCAN reported concentration values for methylene chloride, trichloroethylene, and toluene in the Pinellas ground water were within 20% of reference laboratory values

  1. Electrochromatographic performance of graphene and graphene oxide modified silica particles packed capillary columns.

    Science.gov (United States)

    Zhao, Hongyan; Wang, Yizhou; Zhang, Danyu; Cheng, Heyong; Wang, Yuanchao

    2018-04-01

    Graphene oxide functionalized silica microspheres (GO@SiO 2 ) were synthesized based on condensation reaction between amino from aminosilica particles and carboxyl groups from GO. Reduction of GO@SiO 2 with hydrazinium hydroxide generated graphene modified silica particles (G@SiO 2 ). GO@SiO 2 and G@SiO 2 packed capillary columns for capillary electrochromatography were thereafter fabricated by pressure slurry packing with single-particle frits. GO of 0.3 mg/mL in dispersion solution for GO@SiO 2 synthesis was considered as a compromise between retaining and column efficiency whereas GO@SiO 2 of 20 mg/mL in slurries for column packing was chosen for a homogenous and tight bed. Optimum mobile phases were acquired considering both electroosmotic flow and resolution at an applied voltage of -6 kV as the following: acetonitrile/phosphate buffer (10 mM, pH 7.0), 75:25 (v/v) for polycyclic aromatic hydrocarbons and 50:50 (v/v) for aromatic compounds. A comparison was made between electrochromatographic performances for three PAHs (naphthalene, fluorene and phenanthrene) and three aromatic compounds of various polarities (toluene, aniline and phenol) on bare aminosilica, GO@SiO 2 and G@SiO 2 packed columns, which proved the contribution of alone or combinational actions of solvophobic effect and π-π electron stacking as well as hydrogen bonds to retaining behaviors by GO@SiO 2 and G@SiO 2 . Well over-run, over-day and over-column precisions (retention time: 0.3-1.4, 1.1-3.8 and 2.8-5.2%, respectively; peak area: 2.6-6.5, 4.8-8.3 and 6.5-12.6%, respectively) of GO@SiO 2 packed columns were a powerful proof for good reproducibility. Analytical characteristics of GO@SiO 2 packed capillary columns in CEC analysis of fresh water were evaluated with respect to linearity (R 2 = 0.9961-0.9989) over the range 0.1 to 100 mg/L and detection limits of 9.5 for naphthalene, 12.6 for fluorene and 16.2 μg/L for phenanthrene. Further application to fresh water increased the

  2. Preparation and evaluation of open-tubular capillary column combining a metal-organic framework and a brush-shaped polymer for liquid chromatography.

    Science.gov (United States)

    Chen, Kai; Zhang, Lingyi; Zhang, Weibing

    2018-03-30

    In this work, an open-tubular capillary liquid-phase column was prepared by modifying chain polymer on the inner surface of capillary and chemical bonding of metal organic frameworks, NH 2 -UiO-66, to the brushes of chain polymer (poly(glycidyl methacrylate)). Besides advantages of facial preparation and good permeability, the chain polymer effectively increases the modification amount of NH 2 -UiO-66 nanoparticles to increase the phase ratio of open-tubular capillary column and enhance the interactions with analytes. The results of scanning electron microscope energy-dispersive X-ray spectra indicated that NH 2 -UiO-66 nanoparticles were successfully bonded to the chain polymer. Because of the hydrophobic interaction and hydrogen bonding interaction between the analytes and the ligand of NH 2 -UiO-66, different analytes were well separated on the NH 2 -UiO-66-modified poly(glycidyl methacrylate) capillary (1.12 m × 25 μm id × 365 μm od) with the high absolute column efficiency reaching 121 477 plates, benefiting from an open-tubular column and low mass transfer resistance provided by polymer brush and metal-organic framework crystal. The relative standard deviations of the retention time for run-to-run, day-to-day, and column-to-column (n = 3) runs are below 4.28%, exhibiting good repeatability. Finally, the column was successfully applied to separation of flavonoids in licorice. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

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

    2018-04-01

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

  4. Organics in water contamination analyzer, phase 1

    Science.gov (United States)

    1986-01-01

    The requirements which would result in identifying the components of an automatic analytical system for the analysis of specific organic compounds in the space station potable water supply are defined. The gas chromatographic system for such an analysis is limited to commercially available off-the-shelf hardware and includes the sample inlet, an ionization detector, capillary columns as well as computerized compound identification. The sampling system will be a special variation of the purge and trap Tenax mode using six-port valves and a 500 microliter water sample. Capillary columns used for the separating of contaminants will be bonded phase fused silica with a silicone stationary phase. Two detectors can be used: photoionization and far ultraviolet, since they are sensitive and compatible with capillary columns. A computer system evaluation and program with the principle of compound identification based on the retention index is presented.

  5. Three-Dimensional Numerical Modeling of Acoustic Trapping in Glass Capillaries

    DEFF Research Database (Denmark)

    Ley, Mikkel Wennemoes Hvitfeld; Bruus, Henrik

    2017-01-01

    Acoustic traps are used to capture and handle suspended microparticles and cells in microfluidic applications. A particular simple and much-used acoustic trap consists of a commercially available, millimeter-sized, liquid-filled straight glass capillary actuated by a piezoelectric transducer. Here......, we present a three-dimensional numerical model of the acoustic pressure field in the liquid coupled to the displacement field of the glass wall, taking into account mixed standing and traveling waves as well as absorption. The model explains the dynamical mechanism that leads to the formation...

  6. Temperature-based on-column solute focusing in capillary liquid chromatography reduces peak broadening from pre-column dispersion and volume overload when used alone or with solvent-based focusing.

    Science.gov (United States)

    Groskreutz, Stephen R; Horner, Anthony R; Weber, Stephen G

    2015-07-31

    On-column focusing is essential for satisfactory performance using capillary scale columns. On-column focusing results from generating transient conditions at the head of the column that lead to high solute retention. Solvent-based on-column focusing is a well-known approach to achieve this. Temperature-assisted on-column focusing (TASF) can also be effective. TASF improves focusing by cooling a short segment of the column inlet to a temperature that is lower than the column temperature during the injection and then rapidly heating the focusing segment to the match the column temperature. A troublesome feature of an earlier implementation of TASF was the need to leave the capillary column unpacked in that portion of the column inside the fitting connecting it to the injection valve. We have overcome that problem in this work by packing the head of the column with solid silica spheres. In addition, technical improvements to the TASF instrumentation include: selection of a more powerful thermo-electric cooler to create faster temperature changes and electronic control for easy incorporation into conventional capillary instruments. Used in conjunction with solvent-based focusing and with isocratic elution, volumes of paraben samples (esters of p-hydroxybenzoic acid) up to 4.5-times the column liquid volume can be injected without significant bandspreading due to volume overload. Interestingly, the shapes of the peaks from the lowest volume injections that we can make, 30nL, are improved when using TASF. TASF is very effective at reducing the detrimental effects of pre-column dispersion using isocratic elution. Finally, we show that TASF can be used to focus the neuropeptide galanin in a sample solvent with elution strength stronger than the mobile phase. Here, the stronger solvent is necessitated by the need to prevent peptide adsorption prior to and during analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Controlled crosslinking of trimethylolpropane trimethacrylate for preparation of organic monolithic columns for capillary liquid chromatography.

    Science.gov (United States)

    Gama, Mariana R; Aggarwal, Pankaj; Lee, Milton L; Bottoli, Carla B G

    2017-11-01

    Organic monolithic columns based on single crosslinking of trimethylolpropane trimethacrylate (TRIM) monomer were prepared in a single step by living/controlled free-radical polymerization. Full optimization of the preparation, such as using different percentages of TRIM and different amounts of radical promoter as well as various porogen solvents were explored. The resulting monolithic columns were characterized by scanning electronic microscopy and nitrogen sorption for structure morphology studies and surface area measurements, respectively. Using capillary liquid chromatography, 150 μm i.d. columns were applied to separate a mixture of small hydrophobic molecules. The results indicated that column performance is highly sensitive to the type and the amount of porogen solvents used in the polymerization mixture composition. Good resolution factors and methylene selectivity were obtained, indicating the promising potential of this material for capillary liquid chromatography separations. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Monolithic poly(1,2-bis(p-vinylphenyl)ethane) capillary columns for simultaneous separation of low- and high-molecular-weight compounds.

    Science.gov (United States)

    Greiderer, Andreas; Ligon, S Clark; Huck, Christian W; Bonn, Günther K

    2009-08-01

    Monolithic poly(1,2-bis(p-vinylphenyl)ethane (BVPE)) capillary columns were prepared by thermally initiated free radical polymerisation of 1,2-bis(p-vinylphenyl)ethane in the presence of inert diluents (porogens) and alpha,alpha'-azoisobutyronitrile (AIBN) as initiator. Polymerisations were accomplished in 200 microm ID fused silica capillaries at 65 degrees C and for 60 min. Mercury intrusion porosimetry measurements of the polymeric RP support showed a broad bimodal pore-size-distribution of mesopores and small macropores in the range of 5-400 nm and flow-channels in the mum range. N(2)-adsorption (BET) analysis resulted in a tremendous enhancement of surface area (101 m(2)/g) of BVPE stationary phases compared to typical organic monoliths (approximately 20 m(2)/g), indicating the presence of a considerable amount of mesopores. Consequently, the adequate proportion of both meso- and (small) macropores allowed the rapid and high-resolution separation of low-molecular-weight compounds as well as biomolecules on the same monolithic support. At the same time, the high fraction of flow-channels provided enhanced column permeability. The chromatographic performance of poly(1,2-bis(p-vinylphenyl)ethane) capillary columns for the separation of biomolecules (proteins, oligonucleotides) and small molecules (alkyl benzenes, phenols, phenons) are demonstrated in this article. Additionally, pressure drop versus flow rate measurements of novel poly(1,2-bis(p-vinylphenyl)ethane) capillary columns confirmed high mechanical robustness, low swelling in organic solvents and high permeability. Due to the simplicity of monolith fabrication, comprehensive studies of the retention and separation behaviour of monolithic BVPE columns resulted in high run-to-run and batch-to-batch reproducibilities. All these attributes prove the excellent applicability of monolithic poly(1,2-bis(p-vinylphenyl)ethane) capillary columns for micro-HPLC towards a huge range of analytes of different

  9. 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.

    Science.gov (United States)

    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.

  10. Post-column derivatization capillary electrochromatography for detection of biogenic amines in tuna-meat.

    Science.gov (United States)

    Oguri, Shigeyuki; Okuya, Yukie; Yanase, Yukiko; Suzuki, Sayaka

    2008-08-15

    A system to perform post-column derivatization capillary electrochromatography (CEC) was developed for the first time. The system mainly included a 4-microm (O.D.) silica packed column (200 mm effective length x 0.1 mm inner diameter I.D.) with micro-magnetic particles (MMPs) frits, a T-junction connector, an in-line fluorescence detector and a high-voltage power supply. The system was evaluated by using histamine (HA) as a standard biogenic amine for this study. A 5 microM HA solution was loaded at the anodic site of the capillary column by applying 3 kV for 5s. Then, HA was electrophoretically eluted with a 20mM phosphate buffer (pH 7) by applying 3 kV, and was derivatized with 3mM o-phthalaldehyde (OPA)/N-acetylcysteine (NAC) in 100 mM borate (pH 10), which was continuously delivered through the reagent-loading capillary tube by gravity into the T-junction connector. HA derivative was finally detected with the in-line fluorescence detector (lambda(Ex)=340 nm, lambda(Em)=450 nm) at 9.7 min after sample loading. To test the utility of this system, it was next employed for its ability to detect the presence of HA and other kinds of biogenic amines, including cadaverine (Cad), spermidine (Spm) and tyramine (Tyr) in tuna-meat, once the validity of the method had been confirmed.

  11. A detailed study of CO2-brine capillary trapping mechanisms as applied to geologic carbon storage. Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Wildenschild, Dorthe [Oregon State Univ., Corvallis, OR (United States)

    2017-04-06

    The proposed research focuses on improved fundamental understanding of the efficiency of physical trapping mechanisms, and as such will provide the basis for subsequent upscaling efforts. The overarching hypothesis of the proposed research is that capillary pressure plays a significant role in capillary trapping of CO2, especially during the water imbibition stage of the sequestration process. We posit that the relevant physics of the sequestration process is more complex than is currently captured in relative permeability models, which are often based on so-called trapping models to represent relative permeability hysteresis. Our 4 main questions, guiding the 4 main tasks of the proposed research, are as follows: (1) What is the morphology of capillary trapped CO2 at the pore scale as a function of temperature, pressure, brine concentration, interfacial tension, and pore-space morphology under injection and subsequent imbibition? (2) Is it possible to describe the capillary trapping process using formation-dependent, but otherwise unique continuum-scale functions in permeability-capillary pressure, interfacial area and saturation space, rather than hysteretic functions in permeability-saturation or capillary pressure-saturation space? (3) How do continuum-scale relationships between kr-Pc-S-Anw developed based on pore-scale observations compare with traditional models incorporating relative permeability hysteresis (such as Land’s and other models,) and with observations at the core (5-10cm) scale? (4) How can trapped CO2 volume be optimized via engineered injection and sweep strategies, and as a function of formation type (incl. heterogeneity)?

  12. Capillary pressure - saturation relations in quartz and carbonate sands: Limitations for correlating capillary and wettability influences on air, oil, and supercritical CO2 trapping

    Science.gov (United States)

    Tokunaga, T. K.; Wang, S.; Wan, J.; Dong, W.; Kim, Y.

    2016-12-01

    Capillary pressure (Pc) - saturation (Sw) relations are essential for predicting equilibrium and flow of immiscible fluid pairs in soils and deeper geologic formations. In systems that are difficult to measure, behavior is often estimated based on capillary scaling of easily measured Pc-Sw relations (e.g., air-water, and oil-water), yet the reliability of such approximations needs to be examined. In this study, seventeen sets of brine drainage and imbibition curves were measured with air-brine, decane-brine, and supercritical (sc) CO2-brine in homogeneous quartz and carbonate sands, using porous plate systems under ambient (0.1 MPa, 23 °C) and reservoir (12.0 MPa, 45 °C) conditions. Comparisons between these measurements showed significant differences in residual nonwetting phase saturation, Snw,r. Through applying capillary scaling, changes in interfacial properties were indicated, particularly wettability. With respect to the residual trapping of the nonwetting phases, Snwr, CO2 > Snwr, decane > Snwr, air. Decane-brine and scCO2-brine Pc-Sw curves deviated significantly from predictions assuming hydrophilic interactions. Moreover, neither the scaled capillary behavior nor Snw,r for scCO2-brine were well represented by decane-brine, apparently because of differences in wettability and viscosities, indicating limitations for using decane (and other organic liquids) as a surrogate fluid in studies intended to apply to geological carbon sequestration. Thus, challenges remain in applying scaling for predicting capillary trapping and multiphase displacement processes across such diverse fields as vadose zone hydrology, enhanced oil recovery, and geologic carbon sequestration.

  13. Identification of Aroma Compounds of Lamiaceae Species in Turkey Using the Purge and Trap Technique

    Directory of Open Access Journals (Sweden)

    Ahmet Salih Sonmezdag

    2017-02-01

    Full Text Available The present research was planned to characterize the aroma composition of important members of the Lamiaceae family such as Salvia officinalis, Lavandula angustifolia and Mentha asiatica. Aroma components of the S. officinalis, L. angustifolia and M. asiatica were extracted with the purge and trap technique with dichloromethane and analyzed with the gas chromatography–mass spectrometry (GC–MS technique. A total of 23, 33 and 33 aroma compounds were detected in Salvia officinalis, Lavandula angustifolia and Mentha asiatica, respectively including, acids, alcohols, aldehydes, esters, hydrocarbons and terpenes. Terpene compounds were both qualitatively and quantitatively the major chemical group among the identified aroma compounds, followed by esters. The main terpene compounds were 1,8-cineole, sabinene and linalool in Salvia officinalis, Lavandula angustifolia and Mentha asiatica, respectively. Among esters, linalyl acetate was the only and most important ester compound which was detected in all samples.

  14. Identification of Aroma Compounds of Lamiaceae Species in Turkey Using the Purge and Trap Technique

    Science.gov (United States)

    Sonmezdag, Ahmet Salih; Kelebek, Hasim; Selli, Serkan

    2017-01-01

    The present research was planned to characterize the aroma composition of important members of the Lamiaceae family such as Salvia officinalis, Lavandula angustifolia and Mentha asiatica. Aroma components of the S. officinalis, L. angustifolia and M. asiatica were extracted with the purge and trap technique with dichloromethane and analyzed with the gas chromatography–mass spectrometry (GC–MS) technique. A total of 23, 33 and 33 aroma compounds were detected in Salvia officinalis, Lavandula angustifolia and Mentha asiatica, respectively including, acids, alcohols, aldehydes, esters, hydrocarbons and terpenes. Terpene compounds were both qualitatively and quantitatively the major chemical group among the identified aroma compounds, followed by esters. The main terpene compounds were 1,8-cineole, sabinene and linalool in Salvia officinalis, Lavandula angustifolia and Mentha asiatica, respectively. Among esters, linalyl acetate was the only and most important ester compound which was detected in all samples. PMID:28231089

  15. Preparation of β-cyclodextrin-gold nanoparticles modified open tubular column for capillary electrochromatographic separation of chiral drugs.

    Science.gov (United States)

    Zhou, Li; Jiang, Shenmeng; Zhang, Xue; Fang, Linlin; Guo, Xingjie

    2018-04-01

    In this paper, β-cyclodextrin (β-CD) modified gold nanoparticles (AuNPs) coated open tubular column (OT column) was prepared for capillary electrochromatography. The open tubular column was constructed through self-assembly of gold nanoparticles on 3-mercaptopropyl-trimethoxysilane (MPTMS) prederivatized capillary and subsequent modification of thiols β-cyclodextrin (SH-β-CD). Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and ultraviolet visible spectroscopy were carried out to characterize the prepared open tubular column and synthesized gold nanoparticles. By comparing different coating times of gold nanoparticles and thiols β-cyclodextrin, we got the optimal conditions for preparing the open tubular column. Also, the separation parameters were optimized including buffer pH, buffer concentration and applied voltage. Separation effectiveness of open tubular column was verified by the separation of four pairs of drug enantiomers including bifonazole, fexofenadine, omeprazole and lansoprazole, and satisfactory separation results were achieved for these analytes studied. In addition, the column showed good stability and repeatability. The relative standard deviation values less than 5% were obtained through intra-day, inter-day, and column-to-column investigations. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Pore-scale imaging of capillary trapped supercritical CO2 as controlled by water-wet vs. CO2-wet media and grain shapes

    Science.gov (United States)

    Chaudhary, K.; Cardenas, M.; Wolfe, W. W.; Maisano, J. A.; Ketcham, R. A.; Bennett, P.

    2013-12-01

    The capillary trapping of supercritical CO2 (s-CO2) is postulated to comprise up to 90% of permanently trapped CO2 injected during geologic sequestration. Successive s-CO2/brine flooding experiments under reservoir conditions showed that water-wet rounded beads trapped 15% of injected s-CO2 both as clusters and as individual ganglia, whereas CO2¬-wet beads trapped only 2% of the injected s-CO2 as minute pockets in pore constrictions. Angular water-wet grains trapped 20% of the CO2 but flow was affected by preferential flow. Thus, capillary trapping is a viable mechanism for the permanent CO2 storage, but its success is constrained by the media wettability.

  17. Silica-based monolithic capillary columns modified by liposomes for characterization of analyte–liposome interactions by capillary liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Planeta, Josef; Wiedmer, S. K.

    2013-01-01

    Roč. 1317, SI (2013), s. 159-166 ISSN 0021-9673 R&D Projects: GA MV VG20112015021; GA ČR(CZ) GAP206/11/0138 Institutional support: RVO:68081715 Keywords : monolithic silica capillary column * immobilized liposomes * biomimicking stationary phase Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.258, year: 2013

  18. The hummingbird tongue is a fluid trap, not a capillary tube.

    Science.gov (United States)

    Rico-Guevara, Alejandro; Rubega, Margaret A

    2011-06-07

    Hummingbird tongues pick up a liquid, calorie-dense food that cannot be grasped, a physical challenge that has long inspired the study of nectar-transport mechanics. Existing biophysical models predict optimal hummingbird foraging on the basis of equations that assume that fluid rises through the tongue in the same way as through capillary tubes. We demonstrate that the hummingbird tongue does not function like a pair of tiny, static tubes drawing up floral nectar via capillary action. Instead, we show that the tongue tip is a dynamic liquid-trapping device that changes configuration and shape dramatically as it moves in and out of fluids. We also show that the tongue-fluid interactions are identical in both living and dead birds, demonstrating that this mechanism is a function of the tongue structure itself, and therefore highly efficient because no energy expenditure by the bird is required to drive the opening and closing of the trap. Our results rule out previous conclusions from capillarity-based models of nectar feeding and highlight the necessity of developing a new biophysical model for nectar intake in hummingbirds. Our findings have ramifications for the study of feeding mechanics in other nectarivorous birds, and for the understanding of the evolution of nectarivory in general. We propose a conceptual mechanical explanation for this unique fluid-trapping capacity, with far-reaching practical applications (e.g., biomimetics).

  19. Retention behavior of neutral solutes in pressurized flow-driven capillary electrochromatography using an ODS column.

    Science.gov (United States)

    Nakagawa, Hiroyuki; Kitagawa, Shinya; Araki, Shuki; Ohtani, Hajime

    2006-02-01

    Several alkyl benzenes are separated by pressurized flow-driven capillary electrochromatography using a temperature-controlled capillary column packed with octadecyl siloxane-modified silica gel, and the effect of applied voltage on the retention is investigated. The van't Hoff plot shows good linearity at the column temperature between 305 and 330 K under applications from -6 to +6 kV. The applied voltage causes a relatively large variation in the enthalpy and the entropy of transfer of the solute from the mobile phase to the stationary phase (> 20%). However, the direction of variation in the enthalpy is almost opposite to that in the entropy, both of which might compensate each other. Therefore, the retention factor is not significantly varied (< 4%) by the application of voltage.

  20. Simultaneous determination of eight common odors in natural water body using automatic purge and trap coupled to gas chromatography with mass spectrometry.

    Science.gov (United States)

    Deng, Xuwei; Liang, Gaodao; Chen, Jun; Qi, Min; Xie, Ping

    2011-06-17

    Production and fate of taste and odor (T&O) compounds in natural waters are a pressing environmental issue. Simultaneous determination of these complex compounds (covering a wide range of boiling points) has been difficult. A simple and sensitive method for the determination of eight malodors products of cyanobacterial blooms was developed using automatic purge and trap (P&T) coupled with gas chromatography-mass spectrometry (GC-MS). This extraction and concentration technique is solvent-free. Dimethylsulfide (DMS), dimethyltrisulfide (DMTS), 2-isopropyl-3-methoxypyrazine (IPMP), 2-isobutyl-3-methoxypyrazine (IBMP), 2-methylisoborneol (MIB), β-cyclocitral, geosmin (GSM) and β-ionone were separated within 15.3 min. P&T uses trap #07 and high-purity nitrogen purge gas. The calibration curves of the eight odors show good linearity in the range of 1-500 ng/L with a correlation coefficient above 0.999 (levels=8) and with residuals ranging from approximately 83% to 124%. The limits of detection (LOD) (S/N=3) are all below 1.5 ng/L that of GSM is even lower at 0.08 ng/L. The relative standard deviations (RSD) are between 3.38% and 8.59% (n=5) and recoveries of the analytes from water samples of a eutrophic lake are between 80.54% and 114.91%. This method could be widely employed for monitoring these eight odors in natural waters. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. [Analysis of hydrogen isotopes by gas chromatography using a MnCl2 coated γ-Al2O3 capillary packed column].

    Science.gov (United States)

    Chen, Ping; Fu, Xiaolong; Hu, Peng; Xiao, Chengjian; Ren, Xingbi; Xia, Xiulong; Wang, Heyi

    2017-07-08

    The conventional packed column gas chromatographic analysis of hydrogen isotopes has low column efficiency, broad peak and long retention time. In this work, a γ -Al 2 O 3 with MnCl 2 coated capillary packed column was tested at cryogenic temperature. The systematic column efficiency analysis and the hydrogen isotopes analytical technique research had been carried out. The results showed that, the γ -Al 2 O 3 with MnCl 2 coating could greatly improve the surface degree of order, pore structure and adsorption properties. Also the o -H 2 peak and p -H 2 peak were eluted in a single area. The γ -Al 2 O 3 with MnCl 2 coating was packed into a 0.53 mm inner diameter and 1.0 m long fused silica capillary column. It had a good linear relationship used this column with thermal conductivity detector (TCD) to detect the volume concentrations of hydrogen isotopes from 1 to 10 mL/L, and the relative error was less than 5% for low concentration sample testing. For H 2 , HD and D 2 , the retention times can be shortened to 39, 46 and 60 s, respectively. The limits of detection were reduced to 0.046, 0.067 and 0.072 mL/L, respectively. Compared with conventional packed column, capillary packed column had sharper peak form, higher separation degree of adjacent components, shorter retention time and lower detection limits. The above results indicate that the capillary packed column with TCD detector can be used for fast detection of low concentration of hydrogen isotopes and their online analysis.

  2. Distribution characteristics of volatile methylsiloxanes in Tokyo Bay watershed in Japan: Analysis of surface waters by purge and trap method.

    Science.gov (United States)

    Horii, Yuichi; Minomo, Kotaro; Ohtsuka, Nobutoshi; Motegi, Mamoru; Nojiri, Kiyoshi; Kannan, Kurunthachalam

    2017-05-15

    Surface waters including river water and effluent from sewage treatment plants (STPs) were collected from Tokyo Bay watershed, Japan, and analyzed for seven cyclic and linear volatile methylsiloxanes (VMSs), i.e., D3, D4, D5, D6, L3, L4, and L5 by an optimized purge and trap extraction method. The total concentrations of seven VMSs (ΣVMS) in river water ranged from watershed was estimated at 2300kg. Our results indicate widespread distribution of VMSs in Tokyo Bay watershed and the influence of domestic wastewater discharges as a source of VMSs in the aquatic environment. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. High Efficiency Robust Open Tubular Capillary Electrochromatography Column for the Separation of Peptides

    Energy Technology Data Exchange (ETDEWEB)

    Ali, Faiz; Cheong, Won Jo [Inha University, Incheon (Korea, Republic of)

    2016-08-15

    In this study, the carefully designed tri-component copolymer layer was fabricated onto the inner surface of a pretreated silica capillary (52 cm effective length, 50 μm id). The initiator moieties were incorporated onto the capillary inner surface by reaction with 4-chloromehtylphenyl isocyanate followed by sodium diethyl dithiocarbamate. Next, RAFT copolymerization was held upon the initiator moieties and a thin polymer film was made. The observed peak capacity was, of course, lower than those of the state-of-the art gradient HPLC systems. The UPLC system operated in the long gradient elution mode with a long narrow column of sub-3 μm packed particles could achieve the impressive high peak capacity of ca. 1000. On the other hand, a system with a 20 cm column of 0.8 μm particles could achieve a peak capacity of 220 (comparable to our result) under a pressure of 20 000 psi in a gradient time of 20 min. It should be noted that the operational conditions of this study has been optimized to obtain the best column separation efficiency. It was also operated in the isocratic elution mode. A better peak capacity is expected if the operational conditions are tuned to the optimum peak capacity.

  4. Paleogene stratigraphy of the Solomons Island, Maryland corehole

    Science.gov (United States)

    Gibson, Thomas G.; Bybell, Laurel M.

    1994-01-01

    Purge and trap capillary gas chromatography/mass spectrometry is a rapid, precise, accurate method for determining volatile organic compounds in samples of surface water and ground water. The method can be used to determine 59 selected compounds, including chlorofluorohydrocarbons, aromatic hydrocarbons, and halogenated hydrocarbons. The volatile organic compounds are removed from the sample matrix by actively purging the sample with helium. The volatile organic compounds are collected onto a sorbant trap, thermally desorbed, separated by a Megabore gas chromatographic capillary column, ionized by electron impact, and determined by a full-scan quadrupole mass spectrometer. Compound identification is confirmed by the gas chromatographic retention time and by the resultant mass spectrum. Unknown compounds detected in a sample can be tentatively identified by comparing the unknown mass spectrum to reference spectra in the mass-spectra computer-data system library compiled by the National Institute of Standards and Technology. Method detection limits for the selected compounds range from 0.05 to 0.2 microgram per liter. Recoveries for the majority of the selected compounds ranged from 80 to 120 percent, with relative standard deviations of less than 10 percent.

  5. Preparation and characterization of micro-cell membrane chromatographic column with N-hydroxysuccinimide group-modified silica-based porous layer open tubular capillary.

    Science.gov (United States)

    Xu, Liang; Xu, Bei; Zhao, Zhi-Yu; Yang, Hui-Ping; Tang, Cheng; Dong, Lin-Yi; Liu, Kun; Fu, Li; Wang, Xian-Hua

    2017-09-22

    Cell membrane chromatography (CMC) is an effective tool in screening active compounds from natural products and studying membrane protein interactions. Nevertheless, it always consumes a large amount of cells (e.g. 10 7 -10 8 ) for column preparation. To overcome this, micro-CMC (mCMC), that employs a silica capillary as membrane carrier, was developed. However, both CMC and mCMC suffer from short column life span (e.g. 3days), mainly due to the falling-off of cellular membranes (CMs). This has greatly limited further application of CMC and mCMC, especially when the cells are hard to obtain. To solve this, N-hydroxysuccinimide (NHS)-modified silica-based porous layer open tubular capillary was first prepared for mCMC. The NHS groups can easily react with amino groups on CMs to form a stable covalent bond under a mild condition. So, CMs immobilized on the NHS-modified capillary are less likely to fall off. To verify this, SKBR3/mCMC (Her2 positive) and BALL1/mCMC (CD20 positive) columns were prepared. Two monoclonal antibody drugs, trastuzumab (anti-Her2) and rituximab (anti-CD20), were selected as analytes to characterize the columns. As a result, NHS-modified column for mCMC can afford higher chromatographic retention than non-modified column. Besides, the column life span was significantly improved to more than 16days for SKBR3/mCMC and 14days for BALL1/mCMC, while the compared column showed a sharp decline in retention factor in first 3days. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Pore-scale modeling of capillary trapping in water-wet porous media: A new cooperative pore-body filling model

    Science.gov (United States)

    Ruspini, L. C.; Farokhpoor, R.; Øren, P. E.

    2017-10-01

    We present a pore-network model study of capillary trapping in water-wet porous media. The amount and distribution of trapped non-wetting phase is determined by the competition between two trapping mechanisms - snap-off and cooperative pore-body filling. We develop a new model to describe the pore-body filling mechanism in geologically realistic pore-networks. The model accounts for the geometrical characteristics of the pore, the spatial location of the connecting throats and the local fluid topology at the time of the displacement. We validate the model by comparing computed capillary trapping curves with published data for four different water-wet rocks. Computations are performed on pore-networks extracted from micro-CT images and process-based reconstructions of the actual rocks used in the experiments. Compared with commonly used stochastic models, the new model describes more accurately the experimental measurements, especially for well connected porous systems where trapping is controlled by subtleties of the pore structure. The new model successfully predicts relative permeabilities and residual saturation for Bentheimer sandstone using in-situ measured contact angles as input to the simulations. The simulated trapped cluster size distributions are compared with predictions from percolation theory.

  7. Capillary gas-solid chromatography

    International Nuclear Information System (INIS)

    Berezkin, V.G.

    1996-01-01

    Modern state of gas adsorption chromatography in open capillary columns has been analyzed. The history of the method development and its role in gas chromatography, ways to construct open adsorptional capillary columns, foundations of the theory of retention and washing of chromatographic regions in gas adsorption capillary columns have been considered. The fields is extensively and for analyzing volatile compounds of different isotopic composition, inorganic and organic gases, volatile organic polar compounds, aqueous solutions of organic compounds. Separation of nuclear-spin isomers and isotopes of hydrogen is the first illustrative example of practical application of the adsorption capillary chromatography. It is shown that duration of protium and deuterium nuclear isomers may be reduced if the column temperature is brought to 47 K

  8. A fully automated fast analysis system for capillary gas chromatography. Part 1. Automation of system control

    NARCIS (Netherlands)

    Snijders, H.M.J.; Rijks, J.P.E.M.; Bombeeck, A.J.; Rijks, J.A.; Sandra, P.; Lee, M.L.

    1992-01-01

    This paper is dealing with the design, the automation and evaluation of a high speed capillary gas chromatographic system. A combination of software and hardware was developed for a new cold trap/reinjection device that allows selective solvent eliminating and on column sample enrichment and an

  9. Analysis of polycyclic aromatic hydrocarbons I. Determination by gas chromatography with glass and fused silica capillary columns

    International Nuclear Information System (INIS)

    Perez, M. M.; Gonzalez, D.

    1987-01-01

    A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons is presented. The separation has been carried out by glass and fused silica capillary column. The limitations and the advantages of the procedure are discussed in terms of separation efficiency, sensitivity and precision. (Author) 17 refs

  10. Determination of biodegradation process of benzene, toluene, ethylbenzene and xylenes in seabed sediment by purge and trap gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Han, Dongqiang [Key Lab. for Atomic and Molecular Nanosciences of Education Ministry, Tsinghua Univ., Beijing (China). Dept. of Physics; China Pharmaceutical Univ., Nanjing (China). Physics Teaching and Research Section, Dept. of Basic Sciences; Ma, Wanyun; Chen, Dieyan [Key Lab. for Atomic and Molecular Nanosciences of Education Ministry, Tsinghua Univ., Beijing (China). Dept. of Physics

    2007-12-15

    Benzene, toluene, ethylbenzene, and xylenes (BTEX) are commonly found in crude oil and are used in geochemical investigations as direct indicators of the presence of oil and gas. BTEX are easily volatile and can be degraded by microorganisms, which affect their precise measurement seriously. A method for determining the biodegradation process of BTEX in seabed sediment using dynamic headspace (purge and trap) gas chromatography with a photoionization detector (PID) was developed, which had a detection limit of 7.3-13.2 ng L{sup -1} and a recovery rate of 91.6-95.0%. The decrease in the concentration of BTEX components was monitored in seabed sediment samples, which was caused by microorganism biodegradation. The results of BTEX biodegradation process were of great significance in the collection, transportation, preservation, and measurement of seabed sediment samples in the geochemical investigations of oil and gas. (orig.)

  11. Analysis of polycyclic aromatic hydrocarbons. I. Determination by gas chromatography with glass and fused solica capillary columns

    International Nuclear Information System (INIS)

    Perez Garcia, M.; Gonzalez, D.

    1987-01-01

    A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons is presented. The separation has been carried out by glass and fused silice capillary column. The limitations and the advantages of the procedure are discussed in terms of separation efficiency, sensitivity and precision. (author). 3 figs., 17 refs

  12. Chiral separation of methoxamine and lobeline in capillary zone electrophoresis using ethylbenzene-deactivated fused-silica capillary columns and cyclodextrins as buffer additives.

    Science.gov (United States)

    Russo, M V

    2002-08-01

    The complete chiral separation of methoxamine and lobeline was achieved by capillary zone electrophoresis on an ethylbenzene-deactivated fused-silica capillary column and with cyclodextrins (CDs) as buffer additives. Among the CDs investigated in this study, i.e. alpha-CD, beta-CD, dimethyl-beta-CD, hydroxypropyl-beta-CD and gamma-CD, all the three beta-type CDs showed chiral recognition on the two drugs investigated. Under the investigated conditions, the baseline chiral separation of methoxamine can be achieved with 90 mM Tris-H3PO4 (pH 2.5) containing 11.5 mM of the three beta-type CDs, with dimethyl-beta-CD giving the best resolution, whereas the baseline chiral separation of lobeline can be realized by using 90 mM Tris-H3PO4 buffer (pH 2.5) containing 5.8 mM dimethyl-beta-CD or 29.5 mM hydroxypropyl-beta-CD.

  13. Polydopamine-coated open tubular column for the separation of proteins by capillary electrochromatography.

    Science.gov (United States)

    Xiao, Xing; Wang, Wentao; Chen, Jia; Jia, Li

    2015-08-01

    The separation and determination of proteins in food is an important aspect in food industry. Inspired by the self-polymerization of dopamine under alkaline conditions and the natural adhesive properties of polydopamine, in this paper, a simple and economical method was developed for the preparation of polydopamine-coated open tubular column, in which ammonium persulfate was used as the source of oxygen to induce and facilitate the polymerization of dopamine to form polydopamine. In comparison with a naked fused-silica capillary, the direction and magnitude of the electro-osmotic flow of the as-prepared polydopamine-coated open tubular column could be manipulated by varying the pH values of background solutions due to the existence of amine and phenolic hydroxyl groups on polydopamine coating. The surface morphology of the polydopamine-coated open tubular column was studied by scanning electron microscopy, and the thickness of polydopamine coating was 106 nm. The performance of the polydopamine-coated open tubular column was validated by analysis of proteins. The relative standard deviations of migration times of proteins representing run-to-run, day-to-day, and column-to-column were less than 3.5%. In addition, the feasibility of the polydopamine-coated open tubular column for real samples was verified by the separation of proteins in chicken egg white and pure milk. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Fabrication of single-walled carbon nanohorns incorporated a monolithic column for capillary electrochromatography.

    Science.gov (United States)

    Zhao, Hongyan; Wang, Yizhou; Cheng, Heyong; Wang, Yuanchao

    2017-08-01

    Single-walled carbon nanohorns have received great interest for their unique properties and diverse potential applications. Herein, we demonstrated the feasibility of single-walled carbon nanohorns incorporated poly(styrene-divinylbenzene) monolith as the stationary phase for capillary electrochromatography, which were prepared by one-step in situ copolymerization. Single-walled carbon nanohorns were dispersed in styrene to give a stable and homogeneous suspension. The monolithic column gave effective separation for a wide range of aromatic compounds, which was based on hydrophobicity and π-π electrostatic stacking of single-walled carbon nanohorns. The precisions of migration time and peak area varied in the ranges of 1.4-1.9% for intraday trials and 1.7-3.5% for interday trials, and 3.2-6.7% for intraday trials and 4.1-7.4% for interday trials, and 3.6-7.2% for inter-column trials and 5.2-21.3% for inter-column trials, respectively, indicating the good reproducibility of single-walled carbon nanohorns embedded monolithic columns. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Exploring the effect of mesopore size reduction on the column performance of silica-based open tubular capillary columns.

    Science.gov (United States)

    Hara, Takeshi; Futagami, Shunta; De Malsche, Wim; Baron, Gino V; Desmet, Gert

    2018-06-01

    We report on a modification in the hydrothermal treatment process of monolithic silica layers used in porous-layered open tubular (PLOT) columns. Lowering the temperature from the customary 95 °C to 80 °C, the size of the mesopores reduced by approximately about 35% from 12-13.5 nm to 7.5-9 nm, while the specific pore volume essentially remains unaltered. This led to an increase of the specific surface area (SA) of about 40%, quasi-independent of the porous layer thickness. The increased surface area provided a corresponding increase in retention, somewhat more (48%) than expected based on the increase in SA for the thin layer columns, and somewhat less than expected (34%) for the thick layer columns. The recipes were applied in 5 μm i.d.-capillaries with a length of 60 cm. Efficiencies under retained conditions amounted up to N = 137,000 for the PLOT column with a layer thickness (d f ) of 300 nm and to N = 109,000 for the PLOT column with d f  = 550 nm. Working under conditions of similar retention, the narrow pore/high SA columns produced with the new 80 °C recipe generated the same number of theoretical plates as the wide pore size/low SA columns produced with the 95 °C recipe. This shows the 80 °C-hydrothermal treatment process allows for an increase in the phase ratio of the PLOT columns without affecting their intrinsic mass transfer properties and separation kinetics. This is further corroborated by the fact that the plate height curves generated with the new and former recipe can both be well-fitted with the Golay-Aris equation without having to change the intra-layer diffusion coefficient. Copyright © 2018 Elsevier B.V. All rights reserved.

  16. Analysis of nitrites and nitrates in hams and sausages by open-tubular capillary electrochromatography with a nanolatex-coated capillary column.

    Science.gov (United States)

    Zhang, Yanhao; Tian, Xiangyu; Guo, Yaxiao; Li, Haibin; Yu, Ajuan; Deng, Zhifen; Sun, Barry Baoguo; Zhang, Shusheng

    2014-04-16

    In this work, a new open-tubular capillary electrochromatography (OT-CEC) method with the nanolatex-coated column was proposed for the determination of nitrites and nitrates in foodstuffs. The method was simple and repeatable as a result of avoiding the introduction of an electroosmotic flow reverse additive (such as cetyltrimethylammonium chloride) in electrophoretic buffer. The limits of quantitation were 0.89 and 1.05 mg kg⁻¹ for nitrate and nitrite, respectively, whereas the overall recoveries ranged from 94 to 103%. The developed OT-CEC method was successfully applied for 12 samples, and the residue profiles of nitrites and nitrates in hams and sausages were obtained and evaluated.

  17. Separation and identification of picogram levels of dioxins and PCBs by GC/cryogenic trapping FTIR

    Science.gov (United States)

    Johnson, David J.; Powell, Jay R.; Krishnan, K.

    1994-01-01

    Capillary gas chromatography/mass spectrometry (GC/MS) has routinely been used by the analytical chemist to separate and identify low levels of environmentally important compounds. A GC/Cryogenic Trapping Fourier Transform Infrared Spectrometer (Tracer) provides the sensitivity of the GC/MS with the added capability of differentiating between compounds of the same mass. In this work, the Tracer was utilized to study low levels of six Polychlorinated Biphenyls (PCBs), eight Chlorinated Dibenzo-p-Doxins and Norflurazon. In all cases, picogram levels of these compounds were easily detected from `on the fly' generated IR chromatograms. Since the separated compounds eluting from the capillary column are cryogenically trapped onto a moving liquid nitrogen cooled ZnSe crystal, excellent signal-to- noise spectra of these same compounds may be collected after the run by returning to the same areas of deposition and signal averaging.

  18. Growth of metal-organic framework HKUST-1 in capillary using liquid-phase epitaxy for open-tubular capillary electrochromatography and capillary liquid chromatography.

    Science.gov (United States)

    Bao, Tao; Zhang, Juan; Zhang, Wenpeng; Chen, Zilin

    2015-02-13

    Much attention is being paid to applying metal-organic frameworks (MOFs) as stationary phases in chromatography because of their fascinating properties, such as large surface-to-volume ratios, high levels of porosity, and selective adsorption. HKUST-1 is one of the best-studied face-centered-cubic MOF containing nano-sized channels and side pockets for film growth. However, growth of HKUST-1 framework inside capillary column as stationary phase for capillary electrochromatography is a challenge work. In this work, we carry out the growth of HKUST-1 on the inner wall of capillary by using liquid-phase epitaxy process at room temperature. The fabricated HKUST-1@capillary can be successfully used for the separation of substituted benzene including methylbenzene, ethylbenzene, styrene, chlorobenzene, bromobenzene, o-dichlorobenzene, benzene series, phenolic acids, and benzoic acids derivates. High column efficiency of 1.5×10(5) N/m for methylbenzene was achieved. The formation of HKUST-1 grown in the capillary was confirmed and characterized by scanning electron microscopy images, Fourier transform infrared spectra and X-ray diffraction. The column showed long lifetime and excellent stability. The relative standard deviations for intra-day and inter-day repeatability of the HKUST-1@capillary were lower than 7%. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Shu-Ling; Wang, Chih-Chieh; Fuh, Ming-Ren, E-mail: msfuh@scu.edu.tw

    2016-10-05

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

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

    Science.gov (United States)

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

    2015-08-28

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

  1. On-line purge-and-trap-gas chromatography with flame ionization detection as an alternative analytical method for dimethyl sulphide trace release from marine algae

    Energy Technology Data Exchange (ETDEWEB)

    Careri, M.; Musci, M.; Bianchi, F.; Mucchino, C. [Parma Univ., Parma (Italy). Dipt. di Chimica Generale ed Inorganica, Chimica Analitica e Chimica Fisica; Azzoni, R.; Viaroli, P. [Parma Univ., Parma (Italy). Dipt. di Scienze Ambientali

    2001-10-01

    The release of dimethyl sulphide (DMS) by the seaweed Ulva spp at trace level was studied in aqueous solutions at different salinities, temperature and light intensities. For this purpose, the purge-and-trap technique combined with gas chromatography-flame ionization detection was used. The analytical method was evaluated in terms of linearity range, limit of detection, precision and accuracy by considering 10% (w/v) and 30% (w/v) synthetic seawater as aqueous matrices. Calculation of the recovery function evidenced a matrix influence. The method of standard addition was then used for an accurate determination of DMS in synthetic seawater reproduction the matrix effect. DMS fluxes were analysed in batch cultures of Ulva spp reproducing the conditions which usually occur in the Sacca di Goro lagoon (Northern Adriatic Sea, Italy). [Italian] Il rilascio di dimetilsolfuro (DMS) in tracce da parte della macroalga Ulva spp e' stato studiato in soluzioni acquose di differente salinita' mediante la tecnica purge-and-trap accoppiata on-line alla gascromatografia con rivelazione a ionizzazione di fiamma (GC-FID). Il metodo analitico e' stato validato in termini di linearita' di risposta, di limite di rivelabilita', precisione e accuratezza considerando come matrice acqua di mare sintetica a diversa salinita' (10%0 m/v e 30%0 m/v). Il calcolo della funzione di recupero ha consentito di verificare la presenza di errori sistematici dovuti all'effetto matrice. Il metodo sviluppato e' stato quindi applicato a matrici ambientali allo scopo di verificare il rilascio di DMS da parte di Ulva spp, operando in condizioni ambientali simili a quelle che si verificano nella Sacca di Goro (Ferrara, Italia).

  2. Temperature-assisted On-column Solute Focusing: A General Method to Reduce Pre-column Dispersion in Capillary High Performance Liquid Chromatography

    Science.gov (United States)

    Groskreutz, Stephen R.; Weber, Stephen G.

    2014-01-01

    Solvent-based on-column focusing is a powerful and well known approach for reducingthe impact of pre-column dispersion in liquid chromatography. Here we describe an orthogonal temperature-based approach to focusing called temperature-assisted on-column solute focusing (TASF). TASF is founded on the same principles as the more commonly used solvent-based method wherein transient conditions are created thatlead to high solute retention at the column inlet. Combining the low thermal mass of capillary columns and the temperature dependence of solute retentionTASF is used effectivelyto compress injection bands at the head of the column through the transient reduction in column temperature to 5 °C for a defined 7 mm segment of a 6 cm long 150 μm I.D. column. Following the 30 second focusing time, the column temperature is increased rapidly to the separation temperature of 60 °C releasing the focused band of analytes. We developed a model tosimulate TASF separations based on solute retention enthalpies, focusing temperature, focusing time, and column parameters. This model guides the systematic study of the influence of sample injection volume on column performance.All samples have solvent compositions matching the mobile phase. Over the 45 to 1050 nL injection volume range evaluated, TASF reducesthe peak width for all soluteswith k’ greater than or equal to 2.5, relative to controls. Peak widths resulting from injection volumes up to 1.3 times the column fluid volume with TASF are less than 5% larger than peak widths from a 45 nL injection without TASF (0.07 times the column liquid volume). The TASF approach reduced concentration detection limits by a factor of 12.5 relative to a small volume injection for low concentration samples. TASF is orthogonal to the solvent focusing method. Thus, it canbe used where on-column focusing is required, but where implementation of solvent-based focusing is difficult. PMID:24973805

  3. Temperature-based on-column solute focusing in capillary liquid chromatography reduces peak broadening from precolumn dispersion and volume overload when used alone or with solvent-based focusing

    Science.gov (United States)

    Groskreutz, Stephen R.; Horner, Anthony R.; Weber, Stephen G.

    2015-01-01

    On-column focusing is essential for satisfactory performance using capillary scale columns. On-column focusing results from generating transient conditions at the head of the column that lead to high solute retention. Solvent-based on-column focusing is a well-known approach to achieve this. Temperature-assisted on-column focusing (TASF) can also be effective. TASF improves focusing by cooling a short segment of the column inlet to a temperature that is lower than the column temperature during the injection and then rapidly heating the focusing segment to the match the column temperature. A troublesome feature of an earlier implementation of TASF was the need to leave the capillary column unpacked in that portion of the column inside the fitting connecting it to the injection valve. We have overcome that problem in this work by packing the head of the column with solid silica spheres. In addition, technical improvements to the TASF instrumentation include: selection of a more powerful thermo-electric cooler to create faster temperature changes and electronic control for easy incorporation into conventional capillary instruments. Used in conjunction with solvent-based focusing and with isocratic elution, volumes of paraben samples (esters of p-hydroxybenzoic acid) up to 4.5-times the column liquid volume can be injected without significant bandspreading due to volume overload. Interestingly, the shapes of the peaks from the lowest volume injections that we can make, 30 nL, are improved when using TASF. TASF is very effective at reducing the detrimental effects of precolumn dispersion using isocratic elution. Finally, we show that TASF can be used to focus the neuropeptide galanin in a sample solvent with elution strength stronger than the mobile phase. Here, the stronger solvent is necessitated by the need to prevent peptide adsorption prior to and during analysis. PMID:26091787

  4. Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee bean

    International Nuclear Information System (INIS)

    Zhai, Haiyun; Su, Zihao; Chen, Zuanguang; Liu, Zhenping; Yuan, Kaisong; Huang, Lu

    2015-01-01

    Highlights: • A new GO-MISPE monolithic capillary column was prepared. • The column showed ability of impurities removal and excellent selectivity. • Phloxine B existed in real sample was enriched more than 90 times. • The GO-MISPE column presented good recovery and high stability. • The method was prospered to analyze phloxine B and LOD achieved 0.3 ng g −1 . - Abstract: A method was developed to sensitively determine phloxine B in coffee bean by molecularly imprinted polymers (MIPs) coated graphene oxide (GO) solid-phase extraction (GO-MISPE) coupled with high-performance liquid chromatography and laser-induced fluorescence detection (HPLC–LIF). The GO-MISPE capillary monolithic column was prepared by water-bath in situ polymerization, using GO as supporting material, phloxine B, methacrylic acid (MAA), and ethylene dimethacrylate (EDMA) as template, functional monomer, and cross-linker, respectively. The properties of the homemade GO-MISPE capillary monolithic column, including capacity and specificity, were investigated under optimized conditions. The GO-MIPs were characterized by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy (FT-IR). The mean recoveries of phloxine B in coffee bean ranged from 89.5% to 91.4% and the intra-day and inter-day relative standard deviation (RSD) values all ranged from 3.6% to 4.7%. Good linearity was obtained over 0.001–2.0 μg mL −1 (r = 0.9995) with the detection limit (S/N = 3) of 0.075 ng mL −1 . Under the selected conditions, enrichment factors of over 90-fold were obtained and extraction on the monolithic column effectively cleaned up the coffee bean matrix. The results demonstrated that the proposed GO-MISPE HPLC–LIF method can be applied to sensitively determine phloxine B in coffee bean

  5. Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee bean

    Energy Technology Data Exchange (ETDEWEB)

    Zhai, Haiyun, E-mail: zhaihaiyun@126.com [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China); Su, Zihao [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China); Chen, Zuanguang, E-mail: chenzg@mail.sysu.edu.cn [School of Pharmaceutical Science, Sun Yat-sen University, Guangzhou 510006 (China); Liu, Zhenping; Yuan, Kaisong; Huang, Lu [College of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006 (China)

    2015-03-20

    Highlights: • A new GO-MISPE monolithic capillary column was prepared. • The column showed ability of impurities removal and excellent selectivity. • Phloxine B existed in real sample was enriched more than 90 times. • The GO-MISPE column presented good recovery and high stability. • The method was prospered to analyze phloxine B and LOD achieved 0.3 ng g{sup −1}. - Abstract: A method was developed to sensitively determine phloxine B in coffee bean by molecularly imprinted polymers (MIPs) coated graphene oxide (GO) solid-phase extraction (GO-MISPE) coupled with high-performance liquid chromatography and laser-induced fluorescence detection (HPLC–LIF). The GO-MISPE capillary monolithic column was prepared by water-bath in situ polymerization, using GO as supporting material, phloxine B, methacrylic acid (MAA), and ethylene dimethacrylate (EDMA) as template, functional monomer, and cross-linker, respectively. The properties of the homemade GO-MISPE capillary monolithic column, including capacity and specificity, were investigated under optimized conditions. The GO-MIPs were characterized by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy (FT-IR). The mean recoveries of phloxine B in coffee bean ranged from 89.5% to 91.4% and the intra-day and inter-day relative standard deviation (RSD) values all ranged from 3.6% to 4.7%. Good linearity was obtained over 0.001–2.0 μg mL{sup −1} (r = 0.9995) with the detection limit (S/N = 3) of 0.075 ng mL{sup −1}. Under the selected conditions, enrichment factors of over 90-fold were obtained and extraction on the monolithic column effectively cleaned up the coffee bean matrix. The results demonstrated that the proposed GO-MISPE HPLC–LIF method can be applied to sensitively determine phloxine B in coffee bean.

  6. High-Efficiency On-Line Solid-Phase Extraction Coupling to 15-150 um I.D. Column Liquid Chromatography for Proteomic Analysis

    International Nuclear Information System (INIS)

    Shen, Yufeng; Moore, Ronald J.; Zhao, Rui; Blonder, Josip; Auberry, Deanna L.; Masselon, Christophe D.; Pasa Tolic, Ljiljana; Hixson, Kim K.; Auberry, Kenneth J.; Smith, Richard D.

    2003-01-01

    Flexible manipulation of various properties of proteomic samples is important for proteomic analyses, but it has been little explored for newly developed approaches based on liquid chromatography (LC) in combination with mass spectrometry (MS). With miniaturization of the LC column inner diameter dimensions (required for improving the analysis sensitivity), this issue becomes more challenging due to the small flow rates and the increasing effects of extra column volume on the separation quality and its use for resolving complex proteomic mixtures. In this study, we used commercial switching valves (150-mm channels) to implement the on-line coupling of capillary LC columns with relatively large solid phase extraction (SPE) columns operated at 10,000 psi. With optimized column connections, switching modes, and SPE column dimensions, high-efficiency on-line SPE-capillary and nanoscale LC separations were obtained with peak capacities of ∼1000 for capillaries having inner diameters between 15 to 150 mm. The on-line coupled SPE columns increased the sample processing capabilities by ∼400-fold for sample solution volume and ∼10-fold for sample mass. The proteomic applications of this on-line SPE-capillary LC system were evaluated for analysis of both soluble and membrane protein tryptic digests. Used with an ion trap tandem MS we could typically identify 1100-1500 peptides for analyses in a single 5-hour run. Peptides extracted on the SPE column and eluted from the LC column covered a hydrophilicity/hydrophobicity range that include an estimated ∼98% of all the tryptic peptides. The present implementation also facilitates automation and enables use of both disposable SPE columns and electrospray emitters, providing a robust basis for routine proteomic analyses.

  7. Preparation and evaluation of poly(alkyl methacrylate-co-methacrylic acid-co-ethylene dimethacrylate) monolithic columns for separating polar small molecules by capillary liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Shu-Ling; Wu, Yu-Ru; Lin, Tzuen-Yeuan; Fuh, Ming-Ren, E-mail: msfuh@scu.edu.tw

    2015-04-29

    Highlights: • Methacrylic acid (MAA) was used to increase hydrophilicity of polymeric monoliths. • Fast separation of phenol derivatives was achieved in 5 min using MAA-incorporated column. • Separations of aflatoxins and phenicol antibiotics were achieved using MAA-incorporated column. - Abstract: In this study, methacrylic acid (MAA) was incorporated with alkyl methacrylates to increase the hydrophilicity of the synthesized ethylene dimethacrylate-based (EDMA-based) monoliths for separating polar small molecules by capillary LC analysis. Different alkyl methacrylate–MAA ratios were investigated to prepare a series of 30% alkyl methacrylate–MAA–EDMA monoliths in fused-silica capillaries (250-μm i.d.). The porosity, permeability, and column efficiency of the synthesized MAA-incorporated monolithic columns were characterized. A mixture of phenol derivatives is employed to evaluate the applicability of using the prepared monolithic columns for separating small molecules. Fast separation of six phenol derivatives was achieved in 5 min with gradient elution using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. In addition, the effect of acetonitrile content in mobile phase on retention factor and plate height as well as the plate height-flow velocity curves were also investigated to further examine the performance of the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. Moreover, the applicability of prepared polymer-based monolithic column for potential food safety applications was also demonstrated by analyzing five aflatoxins and three phenicol antibiotics using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column.

  8. Monoliths in capillary electrochromatography and capillary liquid chromatography in conjunction with mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Rantamäki, A. H.; Duša, Filip; Wiedmer, S. K.

    2016-01-01

    Roč. 37, 7-8 (2016), s. 880-912 ISSN 0173-0835 Institutional support: RVO:68081715 Keywords : capillary electrochromatography * capillary liquid chromatography * mass spec- trometry * monolithic columns Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.744, year: 2016

  9. Interactions Between Stratigraphy and Interfacial Properties on Flow and Trapping in Geologic Carbon Storage

    Science.gov (United States)

    Liang, Bo; Clarens, Andres F.

    2018-01-01

    Gas leakage from geologic carbon storage sites could undermine the long-term goal of reducing emissions to the atmosphere and negatively impact groundwater resources. Despite this, there remain uncertainties associated with the transport processes that would govern this leakage. These stem from the complex interaction between governing forces (e.g., gravitational, viscous, and capillary), the heterogeneous nature of the porous media, and the characteristic length scales of these leakage events, all of which impact the CO2 fluid flow processes. Here we assessed how sub-basin-scale horizons in porous media could impact the migration and trapping of a CO2 plume. A high-pressure column packed with two layers of sand with different properties (e.g., grain size and wettability) was used to create a low-contrast stratigraphic horizon. CO2 in supercritical or liquid phase was injected into the bottom of the column under various conditions (e.g., temperature, pressure, and capillary number) and the transport of the resulting plume was recorded using electrical resistivity. The results show that CO2 trapping was most strongly impacted by shifting the wettability balance to mixed-wet conditions, particularly for residual saturation. A 16% increase in the cosine of the contact angle for a mixed-wet sand resulted in nearly twice as much residual trapping. Permeability contrast, pressure, and temperature also impacted the residual saturation but to a lesser extent. Flow rate affected the dynamics of saturation profile development, but the effect is transient, suggesting that the other effects observed here could apply to a broad range of leakage conditions.

  10. Isothermal and non-isothermal infiltration and deuterium transport: a case study in a soil column from a headwater catchment

    Czech Academy of Sciences Publication Activity Database

    Sobotková, M.; Sněhota, M.; Budínová, E.; Tesař, Miroslav

    2017-01-01

    Roč. 65, č. 3 (2017), s. 234-243 ISSN 0042-790X Grant - others:GA ČR(CZ) GA14-03691S Institutional support: RVO:67985874 Keywords : isothermal infiltration * non-isothermal infiltration * column leaching * breakthrough curve * deuterium * viscosity * capillary trapping * entrapped air * permeability Subject RIV: DA - Hydrology ; Limnology OBOR OECD: Environmental sciences (social aspects to be 5.7) Impact factor: 1.654, year: 2016

  11. Determination of butyltin species in natural waters using aqueous phase ethylation and off-line room temperature trapping

    International Nuclear Information System (INIS)

    Bowles, Karl C.; Apte, Simon C.; Hales, Leigh T.

    2003-01-01

    Monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT) were determined in natural water samples by aqueous phase ethylation with sodium tetraethylborate (STEB), room temperature trapping of the resulting volatile derivatives on Tenax TA[reg], followed by gas chromatography-quartz furnace atomic absorption spectrometry (GC-QFAAS). Recoveries of butyltin spikes from natural water samples were 90-109% at concentrations of ∼100 ng Sn/l. The method precision at ∼100 ng Sn/l was ≤6% RSD for butyltins spiked into natural waters. The detection limits for 1 l water samples were <1 ng Sn/l for all butyltin species. Sample throughput of the method is high (greater than three samples per hour) due to the two-stage nature of the procedure, which allows derivatisation/trapping and GC-QFAAS quantitation to be performed separately. Off-line trapping is also advantageous as it extends the life of the GC column and quartz furnace to at least 12 months due to minimisation of carry-over of co-purged material

  12. An experimental study of relative permeability hysteresis, capillary trapping characteristics, and capillary pressure of CO2/brine systems at reservoir conditions

    Science.gov (United States)

    Akbarabadi, Morteza

    We present the results of an extensive experimental study on the effects of hysteresis on permanent capillary trapping and relative permeability of CO2/brine and supercritical (sc)CO2+SO2/brine systems. We performed numerous unsteady- and steady-state drainage and imbibition full-recirculation flow experiments in three different sandstone rock samples, i.e., low and high-permeability Berea, Nugget sandstones, and Madison limestone carbonate rock sample. A state-of-the-art reservoir conditions core-flooding system was used to perform the tests. The core-flooding apparatus included a medical CT scanner to measure in-situ saturations. The scanner was rotated to the horizontal orientation allowing flow tests through vertically-placed core samples with about 3.8 cm diameter and 15 cm length. Both scCO2 /brine and gaseous CO2 (gCO2)/brine fluid systems were studied. The gaseous and supercritical CO2/brine experiments were carried out at 3.46 and 11 MPa back pressures and 20 and 55°C temperatures, respectively. Under the above-mentioned conditions, the gCO2 and scCO2 have 0.081 and 0.393 gr/cm3 densities, respectively. During unsteady-state tests, the samples were first saturated with brine and then flooded with CO2 (drainage) at different maximum flow rates. The drainage process was then followed by a low flow rate (0.375 cm 3/min) imbibition until residual CO2 saturation was achieved. Wide flow rate ranges of 0.25 to 20 cm3/min for scCO2 and 0.125 to 120 cm3min for gCO2 were used to investigate the variation of initial brine saturation (Swi) with maximum CO2 flow rate and variation of trapped CO2 saturation (SCO2r) with Swi. For a given Swi, the trapped scCO2 saturation was less than that of gCO2 in the same sample. This was attributed to brine being less wetting in the presence of scCO2 than in the presence of gCO 2. During the steady-state experiments, after providing of fully-brine saturated core, scCO2 was injected along with brine to find the drainage curve and as

  13. Extreme degree of ionization in homogenous micro-capillary plasma columns heated by ultrafast current pulses.

    Science.gov (United States)

    Avaria, G; Grisham, M; Li, J; Tomasel, F G; Shlyaptsev, V N; Busquet, M; Woolston, M; Rocca, J J

    2015-03-06

    Homogeneous plasma columns with ionization levels typical of megaampere discharges are created by rapidly heating gas-filled 520-μm-diameter channels with nanosecond rise time current pulses of 40 kA. Current densities of up to 0.3  GA cm^{-2} greatly increase Joule heating with respect to conventional capillary discharge Z pinches, reaching unprecedented degrees of ionization for a high-Z plasma column heated by a current pulse of remarkably low amplitude. Dense xenon plasmas are ionized to Xe^{28+}, while xenon impurities in hydrogen discharges reach Xe^{30+}. The unique characteristics of these hot, ∼300:1 length-to-diameter aspect ratio plasmas allow the observation of unexpected spectroscopic phenomena. Axial spectra show the unusual dominance of the intercombination line over the resonance line of He-like Al by nearly an order of magnitude, caused by differences in opacities in the axial and radial directions. These plasma columns could enable the development of sub-10-nm x-ray lasers.

  14. Visualization of residual organic liquid trapped in aquifers

    International Nuclear Information System (INIS)

    Conrad, S.H.; Wilson, J.L.; Mason, W.R.; Peplinski, W.J.

    1992-01-01

    Organic liquids that are essentially immiscible with water migrate through the subsurface under the influence of capillary, viscous, and buoyancy forces. These liquids originate from the improper disposal of hazardous wastes, and the spills and leaks of petroleum hydrocarbons and solvents. The flow visualization experiments described in this study examined the migration of organic liquids through the saturated zone of aquifers, with a primary focus on the behavior of the residual organic liquid saturation, referring to that portion of the organic liquid that is trapped by capillary forces. Etched glass micromodels were used to visually observe dynamic multiphase displacement processes in pore networks. The resulting fluid distributions were photographed. Pore and blob casts were produced by a technique in which an organic liquid was solidified in place within a sand column at the conclusion of a displacement. The columns were sectioned and examined under optical and scanning electron microscopes. Photomicrographs of these sections show the morphology of the organic phase and its location within the sand matrix. The photographs from both experimental techniques reveal that in the saturated zone large amounts of residual organic liquid are trapped as isolated blobs of microscopic size. The size, shape, and spatial distribution of these blobs of residual organic liquid affect the dissolution of organic liquid into the water phase and the biotransformation of organic components. These processes are of concern for the prediction of pollution migration and the design of aquifer remediation schemes

  15. Capillary column switching restricted-access media-liquid chromatography-electrospray ionization-tandem mass spectrometry system for simultaneous and direct analysis of drugs in biofluids.

    Science.gov (United States)

    Santos-Neto, Alvaro J; Markides, Karin E; Sjöberg, Per J R; Bergquist, Jonas; Lancas, Fernando M

    2007-08-15

    Capillary online restricted-access media-liquid chromatography-electrospray ionization-tandem mass spectrometry (RAM-LC-ESI-MS/MS) for direct analysis of drugs and metabolites spiked in biological fluids was developed. Using a column switching setup it was possible to perform effective sample preparation and analysis of raw biological fluids (plasma and urine) without matrix effects in the electrospray mass spectrometric detection step. The peak focusing efficiency of the extraction column was more effective in backflush compared to foreflush mode. The system was able to concentrate diminished samples of polar drugs and their metabolites reaching quantifiable results as low as 1 ng/mL utilizing a sample volume of only 333 nL of biofluids. New column hardware was developed to circumvent clogging problems experienced with plasma injections. The glass fiber filter frit, which is commonly used, was replaced with a short piece of 20 microm i.d. fused silica capillary. The extraction columns were able to handle up to 60 injections and showed a high loading capacity, making the saturation of the MS detector the limiting factor on the linear dynamic range. The simultaneous separation and detection of 10 drugs and metabolites was obtained in 8 min of analysis, including the online sample preparation and enrichment step.

  16. Purged window apparatus utilizing heated purge gas

    Science.gov (United States)

    Ballard, Evan O.

    1984-01-01

    A purged window apparatus utilizing tangentially injected heated purge gases in the vicinity of electromagnetic radiation transmitting windows, and a tapered external mounting tube to accelerate these gases to provide a vortex flow on the window surface and a turbulent flow throughout the mounting tube. Use of this apparatus prevents backstreaming of gases under investigation which are flowing past the mouth of the mounting tube which would otherwise deposit on the windows. Lengthy spectroscopic investigations and analyses can thereby be performed without the necessity of interrupting the procedures in order to clean or replace contaminated windows.

  17. Laser beam trapping and propagation in cylindrical plasma columns

    International Nuclear Information System (INIS)

    Feit, M.D.; Fleck, J.A. Jr.

    1976-01-01

    An analysis of the scheme to heat magnetically confined plasma columns to kilovolt temperatures with a laser beam requires consideration of two propagation problems. The first question to be answered is whether stable beam trapping is possible. Since the laser beam creates its own density profile by heating the plasma, the propagation of the beam becomes a nonlinear phenomenon, but not necessarily a stable one. In addition, the electron density at a given time depends on the preceding history of both the medium and the laser pulse. A self-consistent time dependent treatment of the beam propagation and the medium hydrodynamics is consequently required to predict the behavior of the laser beam. Such calculations have been carried out and indicate that propagation of a laser beam in an initially uniform plasma can form a stable filament which alternately focuses and defocuses. An additional question that is discussed is whether diffractive losses associated with long propagation paths are significant

  18. Capillary Columns with a Sorbent Based on Functionalized Poly(1-Trimethylsilyl-1-Propyne) for the Elution Analysis of Natural Gas

    Science.gov (United States)

    Yakovleva, E. Yu.; Patrushev, Yu. V.; Pai, Z. P.

    2018-05-01

    The chromatographic properties of capillary columns prepared using functionalized poly(1- trimethylsilyl-1-propyne) (PTMSP) are evaluated and compared with the performance of a commercial column with divinylbenzene polymer sorbent. The loading capacity of a PTMSP column with dimensions of 30 m × 0.53 mm × 0.8 μm is shown to be about 2.5 times higher than that of a divinylbenzene polymer column with a diameter of 0.32 mm and a film thickness of 10 μm. The increased value of the background current for PTMSP columns at 220°C is explained by the presence of non-polar bulky substituents in the polymer chain. Differences in the order of elution are found for the following pairs of compounds: acetylene-ethylene; ethane-water; butene-1-isobutane; and sulfur dioxide-carbonyl sulfide. On a column with the functionalized PTMC, analysis of a mixture composition close to natural gas is found to be complete within 27 min.

  19. Direct Analysis of Organic Compounds in Liquid Using a Miniature Photoionization Ion Trap Mass Spectrometer with Pulsed Carrier-Gas Capillary Inlet.

    Science.gov (United States)

    Lu, Xinqiong; Yu, Quan; Zhang, Qian; Ni, Kai; Qian, Xiang; Tang, Fei; Wang, Xiaohao

    2017-08-01

    A miniature ion trap mass spectrometer with capillary direct sampling and vacuum ultraviolet photoionization source was developed to conduct trace analysis of organic compounds in liquids. Self-aspiration sampling is available where the samples are drawn into the vacuum chamber through a capillary with an extremely low flow rate (less than 1 μL/min), which minimizes sample consumption in each analysis to tens of micrograms. A pulsed gas-assisted inlet was designed and optimized to promote sample transmission in the tube and facilitate the cooling of ions, thereby improving instrument sensitivity. A limit of detection of 2 ppb could be achieved for 2,4-dimethylaniline in a methanol solution. The sampling system described in the present study is specifically suitable for a miniature photoionization ion trap mass spectrometer that can perform rapid and online analysis for liquid samples. Graphical Abstract ᅟ.

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

    Science.gov (United States)

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

    2018-07-01

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

  1. Purge ventilation operability

    International Nuclear Information System (INIS)

    Marella, J.R.

    1995-01-01

    A determination of minimum requirements for purge exhaust ventilation system operability has been performed. HLWE and HLW Regulatory Program personnel have evaluated the various scenarios of equipment conditions and HLWE has developed the requirements for purge exhaust systems. This report is provided to document operability requirements to assist Tank Farm personnel to determine whether a system is operable/inoperable and to define required compensatory actions

  2. Integrating reaction and analysis: investigation of higher-order reactions by cryogenic trapping

    Directory of Open Access Journals (Sweden)

    Skrollan Stockinger

    2013-09-01

    Full Text Available A new approach for the investigation of a higher-order reaction by on-column reaction gas chromatography is presented. The reaction and the analytical separation are combined in a single experiment to investigate the Diels–Alder reaction of benzenediazonium-2-carboxylate as a benzyne precursor with various anthracene derivatives, i.e. anthracene, 9-bromoanthracene, 9-anthracenecarboxaldehyde and 9-anthracenemethanol. To overcome limitations of short reaction contact times at elevated temperatures a novel experimental setup was developed involving a cooling trap to achieve focusing and mixing of the reactants at a defined spot in a fused-silica capillary. This trap functions as a reactor within the separation column in the oven of a gas chromatograph. The reactants are sequentially injected to avoid undefined mixing in the injection port. An experimental protocol was developed with optimized injection intervals and cooling times to achieve sufficient conversions at short reaction times. Reaction products were rapidly identified by mass spectrometric detection. This new approach represents a practical procedure to investigate higher-order reactions at an analytical level and it simultaneously provides valuable information for the optimization of the reaction conditions.

  3. Final report of “A Detailed Study of the Physical Mechanisms Controlling CO2-Brine Capillary Trapping in the Subsurface” (University of Arizona, DE-SC0006696)

    Energy Technology Data Exchange (ETDEWEB)

    Schaap, Marcel G. [Univ. of Arizona, Tucson, AZ (United States)

    2016-07-25

    Carbon capture and storage (CCS) of carbon dioxide emissions generated by production or combustion of fossil fuels is a technologically viable means to reduce the build-up of CO2 in the atmosphere and oceans. Using advantages of scale and location, CCS is particularly suitable for large point sources near ubiquitous deep saline aquifers, depleted gas reservoirs, or at production reservoirs for enhanced oil recovery (EOR). In the BES-funded research project, Oregon State University (OSU) carried out capillary trapping experiments with proxy fluids that mimic the properties of the scCO2/brine system under ambient temperatures and pressures, and successfully developed a unique and novel x-ray compatible, high-pressure, elevated temperature setup to study the scCO2/brine system under challenging reservoir conditions. Both methodologies were applied to a variety of porous media, including synthetic (glass bead) and geologic (Bentheimer sandstone) materials. The University of Arizona (UA) developed pore-scale lattice Boltzmann (LB) models which are able to handle the experimental conditions for proxy fluids, as well as the scCO2/brine system, that are capable of simulating permeability in volumes of tens of millions of fluid elements. We reached the following summary findings (main institute indicated): 1. (OSU/UA) To understand capillary trapping in a multiphase fluid-porous medium system, the system must be analyzed from a pore-scale force balance perspective; trapping can be enhanced by manipulating wetting and nonwetting phase fluid properties. 2. (OSU) Pore-scale fluid connectivity and topology has a clear and direct effect on nonwetting phase capillary trapping efficiency. 3. (OSU) Rock type and flow regime also have a pronounced effects on capillary trapping. 4. (OSU/UA) There is a predictable relationship between NWP connectivity and NWP saturation, which allows for development of injection strategies that optimize trapping. The commonly used Land model (Land

  4. The validity and clinical utility of purging disorder.

    Science.gov (United States)

    Keel, Pamela K; Striegel-Moore, Ruth H

    2009-12-01

    To review evidence of the validity and clinical utility of Purging Disorder and examine options for the Diagnostic and Statistical Manual of Mental Disorders fifth edition (DSM-V). Articles were identified by computerized and manual searches and reviewed to address five questions about Purging Disorder: Is there "ample" literature? Is the syndrome clearly defined? Can it be measured and diagnosed reliably? Can it be differentiated from other eating disorders? Is there evidence of syndrome validity? Although empirical classification and concurrent validity studies provide emerging support for the distinctiveness of Purging Disorder, questions remain about definition, diagnostic reliability in clinical settings, and clinical utility (i.e., prognostic validity). We discuss strengths and weaknesses associated with various options for the status of Purging Disorder in the DSM-V ranging from making no changes from DSM-IV to designating Purging Disorder a diagnosis on equal footing with Anorexia Nervosa and Bulimia Nervosa.

  5. Weight-controlled capillary viscometer

    Science.gov (United States)

    Digilov, Rafael M.; Reiner, M.

    2005-11-01

    The draining of a water column through a vertical discharge capillary tube is examined with the aid of a force sensor. The change of the mass of the liquid in the column with time is found to be not purely exponential as implied by Poiseuille's law. Using observed residuals associated with a kinetic energy correction, an approximate formula for the mass as a function of time is derived and excellent agreement with experimental data is attained. These results are verified by a viscosity test of distilled water at room temperature. A simple and inexpensive weight-controlled capillary viscometer is proposed that is especially suitable for undergraduate physics and chemistry laboratories.

  6. Thermodynamics of Capillary Rise: Why Is the Meniscus Curved?

    Science.gov (United States)

    Henriksson, Ulf; Eriksson, Jan Christer

    2004-01-01

    The thermodynamics of capillary rise is explained as the gravitational elevation of the whole column of liquid caused by the positive connection between the liquid, and the solid wall of the capillary tube. The curvature of the meniscus is ascribed to the maintenance of a physiochemical balance throughout the gravitational column of liquid.

  7. Wettability effect on capillary trapping of supercritical CO2 at pore-scale: micromodel experiment and numerical modeling

    Science.gov (United States)

    Hu, R.; Wan, J.

    2015-12-01

    Wettability of reservoir minerals along pore surfaces plays a controlling role in capillary trapping of supercritical (sc) CO2 in geologic carbon sequestration. The mechanisms controlling scCO2 residual trapping are still not fully understood. We studied the effect of pore surface wettability on CO2 residual saturation at the pore-scale using engineered high pressure and high temperature micromodel (transparent pore networks) experiments and numerical modeling. Through chemical treatment of the micromodel pore surfaces, water-wet, intermediate-wet, and CO2-wet micromodels can be obtained. Both drainage and imbibition experiments were conducted at 8.5 MPa and 45 °C with controlled flow rate. Dynamic images of fluid-fluid displacement processes were recorded using a microscope with a CCD camera. Residual saturations were determined by analysis of late stage imbibition images of flow path structures. We performed direct numerical simulations of the full Navier-Stokes equations using a volume-of-fluid based finite-volume framework for the primary drainage and the followed imbibition for the micromodel experiments with different contact angles. The numerical simulations agreed well with our experimental observations. We found that more scCO2 can be trapped within the CO2-wet micromodel whereas lower residual scCO2 saturation occurred within the water-wet micromodels in both our experiments and the numerical simulations. These results provide direct and consistent evidence of the effect of wettability, and have important implications for scCO2 trapping in geologic carbon sequestration.

  8. Costs and Risks of Continuous Purges for Instruments

    Science.gov (United States)

    Secunda, M.; De Garcia, K. Montt

    2018-01-01

    As instruments are built, tested, and launched, they are exposed to environments that have various levels of cleanliness. Often, Scientists and Contamination Control Engineers specify a purge to mitigate the instrument's exposure to a non-clean environment, protect sensitive optics from a specific threat, such as water, or as insurance against things going wrong in a clean environment. The cost of the purge, in effort, dollars and risk, is often understated when the requirements are being established, and the need for purge is not clearly justifiable. This paper will more clearly define some of the costs and risks associated with the continuous purging of instruments during the course of building, testing and launching instruments.

  9. Capillary array electrophoresis using laser-excited confocal fluorescence detection

    Energy Technology Data Exchange (ETDEWEB)

    Huang, X.C.; Quesada, M.A.; Mathies, R.A. [Univ. of California, Berkeley, CA (United States)

    1992-04-15

    Capillary electrophoresis (CE) has found widespread application in analytical and biomedical research, and the scope and sophistication of CE is still rapidly advancing. Gel-filled capillaries have been employed for the rapid separation and analysis of synthetic polynucleotides, DNA sequencing fragments, and DNA restriction fragments. Open-tube capillary electrophoresis has attained subattomole detection levels in amino acid separations 14 and proven its utility for the separation of proteins, viruses, and bacteria. Separation of the optical isomers of dansyl amino acids has also been successfully demonstrated. Micellar electrokinetic capillary chromatography, isoelectric focusing, and on-column derivatization can all be performed on CE columns, demonstrating the utility of capillary electrophoresis as an analytical and micropreparative tool. 29 refs., 6 figs., 1 tab.

  10. Preparation of a β-Cyclodextrin-Based Open-Tubular Capillary Electrochromatography Column and Application for Enantioseparations of Ten Basic Drugs.

    Directory of Open Access Journals (Sweden)

    Linlin Fang

    Full Text Available An open-tubular capillary electrochromatography column was prepared by chemically immobilized β-cyclodextrin modified gold nanoparticles onto new surface with the prederivatization of (3-mercaptopropyl-trimethoxysilane. The synthesized nanoparticles and the prepared column were characterized by transmission electron microscopy, scanning electron microscopy, infrared spectroscopy and ultraviolet visible spectroscopy. When the column was employed as the chiral stationary phase, no enantioselectivity was observed for ten model basic drugs. So β-cyclodextrin was added to the background electrolyte as chiral additive to expect a possible synergistic effect occurring and resulting in a better separation. Fortunately, significant improvement in enantioselectivity was obtained for ten pairs of drug enantiomers. Then, the effects of β-cyclodextrin concentration and background electrolyte pH on the chiral separation were investigated. With the developed separation mode, all the enantiomers (except for venlafaxine were baseline separated in resolutions of 4.49, 1.68, 1.88, 1.57, 2.52, 2.33, 3.24, 1.63 and 3.90 for zopiclone, chlorphenamine maleate, brompheniramine maleate, dioxopromethazine hydrochloride, carvedilol, homatropine hydrobromide, homatropine methylbromide, venlafaxine, sibutramine hydrochloride and terbutaline sulfate, respectively. Further, the possible separation mechanism involved was discussed.

  11. Analysis of bovine milk caseins on organic monolithic columns: an integrated capillary liquid chromatography-high resolution mass spectrometry approach for the study of time-dependent casein degradation.

    Science.gov (United States)

    Pierri, Giuseppe; Kotoni, Dorina; Simone, Patrizia; Villani, Claudio; Pepe, Giacomo; Campiglia, Pietro; Dugo, Paola; Gasparrini, Francesco

    2013-10-25

    Casein proteins constitute approximately 80% of the proteins present in bovine milk and account for many of its nutritional and technological properties. The analysis of the casein fraction in commercially available pasteurized milk and the study of its time-dependent degradation is of considerable interest in the agro-food industry. Here we present new analytical methods for the study of caseins in fresh and expired bovine milk, based on the use of lab-made capillary organic monolithic columns. An integrated capillary high performance liquid chromatography and high-resolution mass spectrometry (Cap-LC-HRMS) approach was developed, exploiting the excellent resolution, permeability and biocompatibility of organic monoliths, which is easily adaptable to the analysis of intact proteins. The resolution obtained on the lab-made Protein-Cap-RP-Lauryl-γ-Monolithic column (270 mm × 0.250 mm length × internal diameter, L × I.D.) in the analysis of commercial standard caseins (αS-CN, β-CN and κ-CN) through Cap-HPLC-UV was compared to the one observe using two packed capillary C4 columns, the ACE C4 (3 μm, 150 mm × 0.300 mm, L × I.D.) and the Jupiter C4 column (5 μm, 150 mm × 0.300 mm, L × I.D.). Thanks to the higher resolution observed, the monolithic capillary column was chosen for the successive degradation studies of casein fractions extracted from bovine milk 1-4 weeks after expiry date. The comparison of the UV chromatographic profiles of skim, semi-skim and whole milk showed a major stability of whole milk towards time-dependent degradation of caseins, which was further sustained by high-resolution analysis on a 50-cm long monolithic column using a 120-min time gradient. Contemporarily, the exact monoisotopic and average molecular masses of intact αS-CN and β-CN protein standards were obtained through high resolution mass spectrometry and used for casein identification in Cap-LC-HRMS analysis. Finally, the proteolytic degradation of β-CN in skim milk

  12. High-Throughput Proteomics Using High Efficiency Multiple-Capillary Liquid Chromatography With On-Line High-Performance ESI FTICR Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shen, Yufeng (BATTELLE (PACIFIC NW LAB)); Tolic, Nikola (BATTELLE (PACIFIC NW LAB)); Zhao, Rui (ASSOC WESTERN UNIVERSITY); Pasa Tolic, Ljiljana (BATTELLE (PACIFIC NW LAB)); Li, Lingjun (Illinois Univ Of-Urbana/Champa); Berger, Scott J.(ASSOC WESTERN UNIVERSITY); Harkewicz, Richard (BATTELLE (PACIFIC NW LAB)); Anderson, Gordon A.(BATTELLE (PACIFIC NW LAB)); Belov, Mikhail E.(BATTELLE (PACIFIC NW LAB)); Smith, Richard D.(BATTELLE (PACIFIC NW LAB))

    2000-12-01

    We report on the design and application of a high-efficiency multiple-capillary liquid chromatography (LC) system for high-throughput proteome analysis. The multiple-capillary LC system was operated at the pressure of 10,000 psi using commercial LC pumps to deliver the mobile phase and newly developed passive feedback valves to switch the mobile phase flow and introduce samples. The multiple-capillary LC system was composed of several serially connected dual-capillary column devices. The dual-capillary column approach was designed to eliminate the time delay for regeneration (or equilibrium) of the capillary column after its use under the mobile phase gradient condition (i.e. one capillary column was used in separation and the other was washed using mobile phase A). The serially connected dual-capillary columns and ESI sources were operated independently, and could be used for either''backup'' operation or with other mass spectrometer(s). This high-efficiency multiple-capillary LC system uses switching valves for all operations and is highly amenable to automation. The separations efficiency of dual-capillary column device, optimal capillary dimensions (column length and packed particle size), suitable mobile phases for electrospray, and the capillary re-generation were investigated. A high magnetic field (11.5 tesla) Fourier transform ion cyclotron resonance (FTICR) mass spectrometer was coupled on-line with this high-efficiency multiple-capillary LC system through an electrospray ionization source. The capillary LC provided a peak capacity of {approx}600, and the 2-D capillary LC-FTICR provided a combined resolving power of > 6 x 10 7 polypeptide isotopic distributions. For yeast cellular tryptic digests, > 100,000 polypeptides were typically detected, and {approx}1,000 proteins can be characterized in a single run.

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

    Science.gov (United States)

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

    2018-02-23

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

  14. In-capillary enrichment, proteolysis and separation using capillary electrophoresis with discontinuous buffers: application on proteins with moderately acidic and basic isoelectric points.

    Science.gov (United States)

    Nesbitt, Chandra A; Yeung, Ken K-C

    2009-01-01

    Advances in mass spectrometry and capillary-format separation continue to improve the sensitivity of protein analysis. Of equal importance is the miniaturization of sample pretreatment such as enrichment and proteolysis. In a previous report (Nesbitt et al., Electrophoresis, 2008, 29, 466-474), nanoliter-volume protein enrichment, tryptic digestion, and partial separation was demonstrated in capillary electrophoresis followed by MALDI mass spectral analysis. A discontinuous buffer system, consisting of ammonium (pH 10) and acetate (pH 4), was used to create a pH junction inside the capillary, trapping a protein with a neutral isoelectric point, myoglobin (pI 7.2). Moreover, co-enrichment of myoglobin with trypsin led to an in-capillary digestion. In this paper, the ability of this discontinuous buffer system to perform similar in-capillary sample pretreatment on proteins with moderately acidic and basic pI was studied and reported. Lentil lectin (pI 8.6) and a multi-phosphorylated protein, beta-casein (pI 5.1), were selected as model proteins. In addition to the previously shown tryptic digestion, proteolysis with endoproteinase Asp-N was also performed. Digestion of these acidic and basic pI proteins produced a few peptides with extreme pI values lying outside the trapping range of the discontinuous buffer. An alteration in the peptide trapping procedure was made to accommodate these analytes. Offline MALDI mass spectral analysis confirmed the presence of the expected peptides. The presented miniaturized sample pretreatment methodology was proven to be applicable on proteins with a moderately wide range of pI. Flexibility in the choice of protease was also evident.

  15. Recent advances in column switching sample preparation in bioanalysis.

    Science.gov (United States)

    Kataoka, Hiroyuki; Saito, Keita

    2012-04-01

    Column switching techniques, using two or more stationary phase columns, are useful for trace enrichment and online automated sample preparation. Target fractions from the first column are transferred online to a second column with different properties for further separation. Column switching techniques can be used to determine the analytes in a complex matrix by direct sample injection or by simple sample treatment. Online column switching sample preparation is usually performed in combination with HPLC or capillary electrophoresis. SPE or turbulent flow chromatography using a cartridge column and in-tube solid-phase microextraction using a capillary column have been developed for convenient column switching sample preparation. Furthermore, various micro-/nano-sample preparation devices using new polymer-coating materials have been developed to improve extraction efficiency. This review describes current developments and future trends in novel column switching sample preparation in bioanalysis, focusing on innovative column switching techniques using new extraction devices and materials.

  16. Purging of working atmospheres inside freight containers.

    Science.gov (United States)

    Braconnier, Robert; Keller, François-Xavier

    2015-06-01

    This article focuses on prevention of possible exposure to chemical agents, when opening, entering, and stripping freight containers. The container purging process is investigated using tracer gas measurements and numerical airflow simulations. Three different container ventilation conditions are studied, namely natural, mixed mode, and forced ventilation. The tests conducted allow purging time variations to be quantified in relation to various factors such as container size, degree of filling, or type of load. Natural ventilation performance characteristics prove to be highly variable, depending on environmental conditions. Use of a mechanically supplied or extracted airflow under mixed mode and forced ventilation conditions enables purging to be significantly accelerated. Under mixed mode ventilation, extracting air from the end of the container furthest from the door ensures quicker purging than supplying fresh air to this area. Under forced ventilation, purging rate is proportional to the applied ventilation flow. Moreover, purging rate depends mainly on the location at which air is introduced: the most favourable position being above the container loading level. Many of the results obtained during this study can be generalized to other cases of purging air in a confined space by general ventilation, e.g. the significance of air inlet positioning or the advantage of generating high air velocities to maximize stirring within the volume. © The Author 2015. Published by Oxford University Press on behalf of the British Occupational Hygiene Society.

  17. Plasma L-ergothioneine measurement by high-performance liquid chromatography and capillary electrophoresis after a pre-column derivatization with 5-iodoacetamidofluorescein (5-IAF) and fluorescence detection.

    Science.gov (United States)

    Sotgia, Salvatore; Pisanu, Elisabetta; Pintus, Gianfranco; Erre, Gian Luca; Pinna, Gerard Aime; Deiana, Luca; Carru, Ciriaco; Zinellu, Angelo

    2013-01-01

    Two sensitive and reproducible capillary electrophoresis and high-performance liquid chromatography-fluorescence procedures were established for quantitative determination of L-egothioneine in plasma. After derivatization of L-ergothioneine with 5-iodoacetamidofluorescein, the separation was carried out by HPLC on an ODS-2 C-18 sperisorb column by using a linear gradient elution and by HPCE on an uncoated fused silica capillary, 50 µm id, and 60 cm length. The methods were validated and found to be linear in the range of 0.3 to 10 µmol/l. The limit of quantification was 0.27 µmol/l for HPCE and 0.15 µmol/l for HPLC. The variations for intra- and inter-assay precision were around 6 RSD%, and the mean recovery accuracy close to 100% (96.11%).

  18. Regioselective photoamination of 4-nitroveratrole upon cyclodextrin ...

    Indian Academy of Sciences (India)

    Unknown

    irradiated for 6 h in the same reactor after purging with nitrogen gas for 30 min. ... by gas chromatography (Shimadzu 17A) using SE-30 10% capillary column, FID .... CD complex with 3 in solution yields the para-substituted compound 3c as ...

  19. Gas-chromatographic separation of hydrogen isotopes mixtures on capillary molecular sieve 5 A column at 173 K

    International Nuclear Information System (INIS)

    Bidica, N.; Preda, A.; Stanciu, V.

    2002-01-01

    Analysis of a gas mixture of hydrogen species, is not too easy because the differences in their physical-chemical properties are very small; the most different are their masses, and consequently most common analytical method appear to be the mass-spectrometry. However, the impossibility to distinguish between two ions (atomic or molecular) with the same mass renders this method as unapplicable. Another problem is the decay of tritium with production of 3 He. These disadvantages of mass-spectrometry have made that other analytical methods, like gas chromatography, to be considered and developed. Thus, there are many papers about various chromatographic columns especially prepared for hydrogen species separation but the preparation and treatment of these columns are very difficult to reproduce. Besides these, there are two other main disadvantages: column operating temperature is very low and long retention times for hydrogen species (more than half an hour) are required. However, the gas-chromatography method still remains an appropriate one. The method described in this paper was based on using a capillary molecular sieve 5A column which has been operated for this kind of separation. The retention times were relatively short, about 8-9 minutes. The carrier gas was Ne and the detector - TCD. In the paper chromatograms for various carrier flow rates and various hydrogen isotope mixtures are presented. The results demonstrated a quite good efficiency for H 2 , HD, D 2 and a not very good one for orthoH 2 -paraH 2 . (authors)

  20. Purging behavior in anorexia nervosa and eating disorder not otherwise specified

    DEFF Research Database (Denmark)

    Støving, René Klinkby; Andries, Alin; Brixen, Kim Torsten

    2012-01-01

    Purging behavior in eating disorders is associated with medical risks. We aimed to compare remission rates in purging and non-purging females with anorexia nervosa (AN) and eating disorder not otherwise specified (EDNOS) in a large retrospective single center cohort. A total of 339 patients...

  1. Estimation of tritium trapped in the used ion exchange column resins using water as scavenger

    International Nuclear Information System (INIS)

    Kumaravel, S.; Ramakrishna, V.; Nair, B.S.K.; Ganesh, G.; Tripathi, R.M.

    2018-01-01

    Estimation of Tritium trapped in the used resins of Ion exchange (IX) columns apart from the gross beta activity in heavy water systems of Pressurised Heavy Water Reactors (PHWR) is mandatory before their disposal as radioactive waste. The gross beta activity is estimated by Gieger- Muller (GM) counter and by using gamma spectrometer. Accurate estimation of tritium activity of the resin without compromising the counting efficiency is a challenging task because, if a fixed quantity of the resin is directly added to the scintillation solution and counted on a liquid scintillation analyser (LSA), it is prone to interfere with counting efficiency drastically and results in unquantifiable errors and other practical difficulties. In this study a standard technique using light water as scavenger medium to precisely quantify the total activity of tritium trapped in the resin by a systematic approach was carried out

  2. Preparation of a long-alkyl-chain-based hybrid monolithic column with mixed-mode interactions using a "one-pot" process for pressurized capillary electrochromatography.

    Science.gov (United States)

    Lyu, Haixia; Zhao, Heqing; Qin, Wenfei; Xie, Zenghong

    2017-12-01

    A simple "one-pot" approach for the preparation of a new vinyl-functionalized organic-inorganic hybrid monolithic column is described. In this improved method, the hydrolyzed alkoxysilanes of tetramethoxysilane and triethoxyvinylsilane were used as precursors for the synthesis of a silica-based monolith, while 1-hexadecene and sodium ethylenesulfonate were used as vinyl functional monomers along with azobisisobutyronitrile as an initiator. The effects of reaction temperature, urea content, and composition of organic monomers on the column properties (e.g. morphology, mechanical stability, and chromatographic performance) were investigated. The monolithic column was used for the separation of neutral solutes by reversed-phase pressurized capillary. Furthermore, the monolith can separate various aromatic amines, which indicated its excellent cation-exchange capability and hydrophobic interactions. The baseline separation of the aromatic amines was obtained with a column efficiency of up to 78 000 plates/m. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Flow rate control in pressure-programmed capillary supercritical fluid chromatography

    NARCIS (Netherlands)

    Janssen, J.G.M.; Rijks, J.A.; Cramers, C.A.M.G.

    1990-01-01

    A versatile and simple system is described that allows variation of the column flow rate in open-tubular capillary supercritical fluid chromatography using both on-column and postcolumn detection. The system is based on column-effluent splitting in a low-dead-volume T piece at the column exit just

  4. Trihalomethanes in potable water

    International Nuclear Information System (INIS)

    Ahmad, M.; Bajahalan, A.S.

    2005-01-01

    These experiments were conducted to evaluate the quality of potable water in Yanbu AI-Sinaiyah, one of the leading industrial city in the Kingdom of Saudi Arabia. The major source of water is Redsea. Desalinated water is distributed in the whole city for domestic uses. At the treatment plant chlorine is being used as disinfectant in pre and post desalination. The present study was conducted to determine the presence of disinfection by-products in potable water. Trihalomethanes are the major disinfection by-products found in the chlorinated water. Trihalomethanes identified in these experiments are chloroform, dichlorobromomethane, dibromochloromethane and tribromomethane. Thichloromethanes are considered to be carcinogenic, hence it is very important to investigate the presence of these compounds in potable water. Samples were collected from consumers tap and preserved at the site for analysis. In the laboratory samples were extracted by Tekmar Velocity XPT purge and trap unit. High purity nitrogen was purged through a sparger in the samples and purged volatiles were trapped in a carbo trap at room temperature. Then trapped components were desorbed with high purity helium and transferred to gas chromatograph injector and analysed by Varian Saturn 2200 GC-MS using 30 m long factor four capillary column. The effect of temperature and seasonal variation (winter and summer) was also monitored. Mean trihalomethane level was higher in summer (8.617 micro g/L) than in winter (5.173 micro g/L). Mean concentration of all the four THMs was 6.9 micro g/L, much less than prescribed EPA limits (80 micro g/L). About 13 brands of bottled water were also analysed for THMs. Only tribromomethane and dibromochloromethane were detected in few brands. Experiments were also conducted to remove THMs from chlorinated water and found that passing through activated charcoal and boiling the water for couple of minutes were sufficient to remove all the THMs from chlorinated water. (author)

  5. Quality assurance plan for the Molten Salt Reactor Experiment Remediation Project at the Oak Ridge National Laboratory. Phase 1 -- Interim corrective measures and Phase 2 -- Purge and trap reactive gases

    International Nuclear Information System (INIS)

    1995-11-01

    This Quality Assurance Plan (QAP) identifies and describes the systems utilized by the Molten Salt Reactor Experiment Remediation Project (MSRERP) personnel to implement the requirements and associated applicable guidance contained in the Quality Program Description Y/QD-15 Rev. 2 (Energy Systems 1995f). This QAP defines the quality assurance (QA) requirements applicable to all activities and operations in and directly pertinent to the MSRERP Phase 1--Interim Corrective Measures and Phase 2--Purge and Trap objectives. This QAP will be reviewed, revised, and approved as necessary for Phase 3 and Phase 4 activities. This QAP identifies and describes the QA activities and procedures implemented by the various Oak Ridge National Laboratory support organizations and personnel to provide confidence that these activities meet the requirements of this project. Specific support organization (Division) quality requirements, including the degree of implementation of each, are contained in the appendixes of this plan

  6. Analytical biotechnology: Capillary electrophoresis and chromatography

    International Nuclear Information System (INIS)

    Horvath, C.; Nikelly, J.G.

    1990-01-01

    The papers describe the separation, characterization, and equipment required for the electrophoresis or chromatography of cyclic nucleotides, pharmaceuticals, therapeutic proteins, recombinant DNA products, pheromones, peptides, and other biological materials. One paper, On-column radioisotope detection for capillary electrophoresis, has been indexed separately for inclusion on the data base

  7. [Purging behaviors and nutritional status in anorexia nervosa and bulimia nervosa].

    Science.gov (United States)

    Vaz, F J; García-Herráiz, A; López-Vinuesa, B; Monge, M; Fernández-Gil, M A; Guisado, J A

    2003-01-01

    The aim of the study was to investigate whether the use of purgative methods in patients with eating disorders (anorexia nervosa [AN] and bulimia nervosa [BN]) could be capable of producing changes in the nutritional status of the patients. The group under study was composed of 184 female eating disordered outpatients. One hundred and sixteen patients (63.0%) fulfilled the DSM-IV diagnostic criteria for BN (90 purging type, 26 nonpurging type). Sixty eight patients (37.0%) fulfilled the DSM-IV criteria for the diagnosis of AN (48 restricting type, 20 binging-purging type). The assessment process included anthropometry (body circumferences and skinfold thickness) and body impedance analysis. The two subgroups of AN patients significantly differed from each of the BN subgroups. From a nutritional point of view, some significant differences between the two DSM-IV subtypes of AN existed, but not between the purging type and the nonpurging type of BN. The paper discusses the clinical significance of these findings. An alternative subtypification of AN patients is proposed: 1) restricting type [patients who control their food intake and do not purge]; 2) purging type [patient with true episodes of binging which are followed by purgative behaviors]; and 3) pseudopurging type [patients with subjective binging episodes who use purging methods].

  8. Characterization of oligosaccharides with capillary high performance anion exchange chromatography hyphenated to pulsed amperometric detection and ion trap mass spectrometry : application to the analysis of human lysosomal disorders

    NARCIS (Netherlands)

    Bruggink, Cornelis

    The development of a capillary ion chromatograph is described together with a matching desalter. This desalter made it possible to use on-line a mass spectrometer. The mass spectrometer enables partly to characterize carbohydrates eluting from the anion exchange column. This separation technology is

  9. Chromatographic efficiency of polar capillary columns applied for the analysis of fatty acid methyl esters by gas chromatography.

    Science.gov (United States)

    Waktola, Habtewold D; Mjøs, Svein A

    2018-04-01

    The chromatographic efficiency that could be achieved in temperature-programmed gas chromatography was compared for four capillary columns that are typically applied for analysis of fatty acid methyl esters (FAME). Three different carrier gases, hydrogen, helium and nitrogen, were applied. For each experiment, the carrier gas velocities and the temperature rates were varied with a full 9 × 3 design, with nine levels on the carrier gas velocity and temperature rates of 1, 2 or 3°C/min. Response surface methodology was used to create models of chromatographic efficiency as a function of temperature rate and carrier gas velocity. The chromatographic efficiency was defined as the inverse of peak widths measured in retention index units. The final results were standardized so that the efficiencies that could be achieved within a certain time frame, defined by the retention time of the last compound in the chromatogram, could be compared. The results show that there were clear differences in the efficiencies that could be achieved with the different columns and that the efficiency decreased with increasing polarity of the stationary phase. The differences can be explained by higher resistance to mass transfer in the stationary phase in the most polar columns. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Simultaneous determination of metoprolol and metabolites in urine by capillary column gas chromatography as oxazolidineone and trimethylsilyl derivatives.

    Science.gov (United States)

    Gyllenhaal, O; Hoffmann, K J

    1984-08-10

    A method for the determination of metoprolol and its main metabolites in urine is presented. The method comprises derivatization of the aminopropanol side-chain with phosgene at alkaline pH and isolation in an organic phase at acidic pH. After trimethylsilylation, separation and quantification are performed by capillary column gas chromatography with flame ionization detection. The reaction is performed at pH 12 with 60 microliters of 2 M phosgene in toluene added in three portions. Diethyl ether--dichloromethane is used as extraction medium and bis(trimethylsilyl) acetamide as silylating agent. With spiked samples linear standard curves were obtained for metoprolol and three of its main metabolites with a detection limit varying between 4 and 20 mumol/l of urine. The method was applied to urine samples from a normal individual who had taken 292 mumol of metoprolol as tartrate.

  11. Programmed temperature vaporizing injector to filter off disturbing high boiling and involatile material for on-line high performance liquid chromatography gas chromatography with on-column transfer.

    Science.gov (United States)

    Biedermann, Maurus; Grob, Koni

    2013-03-15

    Insertion of a programmed temperature vaporizing (PTV) injector under conditions of concurrent solvent recondensation (CSR) into the on-line HPLC-GC interface for on-column transfer (such as the retention gap technique with partially concurrent eluent evaporation) enables filtering off high boiling or involatile sample constituents by a desorption temperature adjusted to the required cut-off. Details of this technique were investigated and optimized. Memory effects, observed when transferred liquid was sucked backwards between the transfer line and the wall of the injector liner, can be kept low by a small purge flow rate through the transfer line at the end of the transfer and the release of the liquid through a narrow bore capillary kept away from the liner wall. The column entrance should be within the well heated zone of the injector to prevent losses of solute material retained on the liner wall during the splitless period. The desorption temperature must be maintained until an elevated oven temperature is reached to prevent peak broadening resulting of a cool inlet section in the bottom part of the injector. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Volatile hydrocarbon profile of Iberian dry-cured hams. A possible tool for authentication of hams according to the fattening diet.

    Science.gov (United States)

    Narváez-Rivas, Mónica; Vicario, Isabel M; Alcalde, M Jesús; León-Camacho, Manuel

    2010-06-15

    The aims of this work were to carry out a comprehensive study of the volatile hydrocarbons of 34 Iberian dry-cured hams and to evaluate the efficiency of these compounds for discriminating hams according to the fattening system: "Montanera" (B) and "Cebo" (C). The samples of hams were obtained by mincing the semimembranosus and semitendinosus muscles from slices of dry-cured ham. The analyses were carried out by gas chromatography-mass spectrometry with a polar capillary column and after a previous extraction by Purge and Trap method. Forty-three volatile hydrocarbons were identified, 26 of them for the first time in Iberian dry-cured ham. Only five compounds showed significant differences between the two types of hams. Among the 33 volatile hydrocarbons, 22 of them allowed a complete discrimination of the two groups of hams according the fattening system.

  13. Development of a positive column pulsed capillary discharge source for use with high resolution Fourier transform spectrometer

    International Nuclear Information System (INIS)

    Syed, W A A

    2002-01-01

    We report the designing and application of a positive column pulsed capillary discharge with the Fourier transform spectrometer (FTS). The pulsed light source has been used for the first time with the ultraviolet FTS. The experiment has been carried out with the high energy pulsed discharge with energy of 2-3 J lasting about 300 ns. A system has been developed to trigger the discharge at about 600 Hz with the pulses directly taken from the FTS sampling system. The spectrum of Ar III has been recorded in the 19 000-50 000 cm -1 region with good signal to noise ratio. The results have opened a wide range of applications in spectroscopy of multiply ionized species

  14. Evaluation of Carbon Nanotubes Functionalized Polydimethylsiloxane Based Coatings for In-Tube Solid Phase Microextraction Coupled to Capillary Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Neus Jornet-Martínez

    2015-08-01

    Full Text Available In the present work, the performance of carbon nanotubes (c-CNTs functionalized polydimethylsiloxane (PDMS based coatings as extractive phases for in-tube solid phase microextraction (IT-SPME coupled to Capillary LC (CapLC has been evaluated. Carboxylic-single walled carbon nanotubes (c-SWNTs and carboxylic-multi walled carbon nanotubes (c-MWNTs have been immobilized on the activated surface of PDMS capillary columns. The effect of different percentages of diphenyl groups in the PDMS extractive phase has also been evaluated. The extraction capability of the capillary columns has been tested for different organic pollutants, nitrogen heterocyclic compounds and polycyclic aromatic compounds (PAHs. The results indicated that the use of the c-CNTs-PDMS capillary columns improve pyriproxyfen and mainly PAH extraction. Triazines were better extracted by unmodified TRB-35 and modified c-CNTs-PDMSTRB-5. The results showed that the extraction capability of the c-CNT capillary columns depends not only on the polarity of the analytes (as it occurs with PDMS columns but also on the interactions that the analytes can establish with the immobilized c-CNTs on the PDMS columns. The extraction efficiency has been evaluated on the basis of the preconcentration rate that can be achieved, and, in this sense, the best c-CNTs-PDMS capillary column for each group of compounds can be proposed.

  15. A selective and sensitive method for quantitation of lysergic acid diethylamide (LSD) in whole blood by gas chromatography-ion trap tandem mass spectrometry.

    Science.gov (United States)

    Libong, Danielle; Bouchonnet, Stéphane; Ricordel, Ivan

    2003-01-01

    A gas chromatography-ion trap tandem mass spectrometry (GC-ion trap MS-MS) method for detection and quantitation of LSD in whole blood is presented. The sample preparation process, including a solid-phase extraction step with Bond Elut cartridges, was performed with 2 mL of whole blood. Eight microliters of the purified extract was injected with a cold on-column injection method. Positive chemical ionization was performed using acetonitrile as reagent gas; LSD was detected in the MS-MS mode. The chromatograms obtained from blood extracts showed the great selectivity of the method. GC-MS quantitation was performed using lysergic acid methylpropylamide as the internal standard. The response of the MS was linear for concentrations ranging from 0.02 ng/mL (detection threshold) to 10.0 ng/mL. Several parameters such as the choice of the capillary column, the choice of the internal standard and that of the ionization mode (positive CI vs. EI) were rationalized. Decomposition pathways under both ionization modes were studied. Within-day and between-day stability were evaluated.

  16. Characterisation of capillary ionic liquid columns for gas chromatography-mass spectrometry analysis of fatty acid methyl esters.

    Science.gov (United States)

    Zeng, Annie Xu; Chin, Sung-Tong; Nolvachai, Yada; Kulsing, Chadin; Sidisky, Leonard M; Marriott, Philip J

    2013-11-25

    Due to their distinct chemical properties, the application of ionic liquid (IL) compounds as gas chromatography (GC) stationary phases offer unique GC separation especially in the analysis of geometric and positional fatty acid methyl ester (FAME) isomers. Elution behaviour of FAME on several commercialised IL capillary columns including phosphonium based SLB-IL59, SLB-IL60, SLB-IL61 and SLB-IL76 and imidazolium based SLB-IL82, SLB-IL100, and SLB-IL111 as well as a general purpose column SLB-5ms, were evaluated in gas chromatography-mass spectrometry (GC-MS) analysis. The phases were further characterised by using a linear solvation energy relationship (LSER) approach according to the equivalent chain length (ECL) index of FAME. Among all tested IL columns, elution temperatures of saturated FAME increased as their McReynolds' polarity value decreased, except for IL60. ECL values increased markedly as the stationary phase polarity increased, particularly for the polyunsaturated FAME. The LSER study indicated a lowest l/e value at 0.864 for IL111, displaying phase selectivity towards unsaturated FAME, with higher peak capacity within a carbon number isomer group. s and e descriptors calculated from LSER were validated by excellent correlation with dipole moments and lowest unoccupied molecular orbital (LUMO) energies, with R(2) values of 0.99 and 0.92 respectively, calculated using GAUSSIAN. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. The Phillips Laboratory capillary pumped loop test facility

    Science.gov (United States)

    Gluck, Donald F.; Kaylor, Marc C.

    1996-03-01

    An ammonia capillary pumped loop (CPL) test facility has been designed, fabricated, subject to acceptance tests, and assembled at Phillips Laboratory. Its intent is to support a wide range of Air Force programs, bringing CPL technology to flight readiness for operational systems. The facility provides a high degree of modularity and flexibility with several heating and cooling options, and capability for elevation (+/- 15 in.), tilt (+/-60°) and transport length variation. It has a 182 by 44 by 84 inch envelope, an expected heat load capability of 2500 W, and a temperature range of 0 to 50 °C. The evaporator section has two plates with four capillary pumps (CPs) each, with a starter pump on one plate. The CPs are 5/8 in., with TAG aluminum 6063-T6 casing and UHMW polyethylene wicks. The active lengths are 15 and 30 inch with both 10 and 15 micron wicks. The individual CPs have thermal and hydraulic isolation capability, and are removable. The transport section consists of stainless steel lines in a serpentine configuration, a 216 in3 free volume reservoir, and a mechanical pump. The vapor transport line contains a capillary device (which can be bypassed) for vapor blockage during startup. The condenser consists of two separately valved, parallel cold plates each with a downstream noncondensible gas trap. Cooling of up to 1500 W at -50 °C is provided by an FTS Systems chiller using Flourinert FC-72. An enclosure/exhaust system is provided for safety and emergency venting of ammonia. An ammonia charge station performs or supports the functions of proof pressure, flushing with ammonia, purging with gaseous nitrogen, evacuation of all or part of the CPL to 20 microns, and charging. Instrumentation consists of over 116 thermocouples, five of which are internal; one absolute and six differential pressure transducers; eleven watt transducers, and a reservoir load cell. The data acquisition system consists of a temperature scanner, Bernoulli drive, and two Macintosh

  18. Qualitative and quantitative analysis of cations and anions using ion selective detectors in capillary electrophoresis

    International Nuclear Information System (INIS)

    Nann, A.

    1994-01-01

    The present work reports on the application of ion-selective microelectrodes as potentiometric detectors for the qualitative and quantitative analysis of cations and anions separated by capillary electrophoresis. Due to the high internal resistance of microelectrodes, their potentials are strongly affected by external electrical fields. Therefore, the influence of the electrophoretic field on the electrode response had to be kept at a minimum. With the electrode tip inserted in the capillary aperture (on-column detection), heavy drifts and noise of the signals were observed, mainly because the electrophoretic potential is superimposed on the Nernstian electrode response. As the potential inside the capillary is site-dependent, already minor movements and vibrations not perceptible under the light microscopy cause unacceptable disturbances of the electrode signal. One possibility to solve the problem consists in post- or off-column detection, i.e., with the detector located outside the influence of the electrophoretic field. If quantitative analyses with maximum resolution are to be achieved, only on-column detection is suitable because outside the capillary, the separation efficiency drops drastically. By etching the detector-side capillary end to a conical aperture, the field strength in the last 10 μm fell approximately 1/25 as compared with that in a cylindrical one. Thus, potential drifts and noise were reduced correspondingly so that on-column detection can also be used for potentiometric detection. To obtain quantitative results, the signals of the ion-selective detector were first delogarithmized and then integrated over time. Thus, it was possible to quantify cations and anions with a coefficient of variations ≤5%. (author) figs., tabs., 179 refs

  19. Ion-pair in-tube solid-phase microextraction and capillary liquid chromatography using a titania-based column: application to the specific lauralkonium chloride determination in water.

    Science.gov (United States)

    Prieto-Blanco, M C; Moliner-Martínez, Y; López-Mahía, P; Campíns-Falcó, P

    2012-07-27

    A quick, miniaturized and on-line method has been developed for the determination in water of the predominant homologue of benzalkonium chloride, dodecyl dimethyl benzyl ammonium chloride or lauralkonium chloride (C(12)-BAK). The method is based on the formation of an ion-pair in both in-tube solid-phase microextraction (IT-SPME) and capillary liquid chromatography. The IT-SPME optimization required the study of the length and nature of the stationary phase of capillary and the processed sample volume. Because to the surfactant character of the analyte both, the extracting and replacing solvents, have played a decisive role in the IT-SPME optimized procedure. Conditioning the capillary with the mobile phase which contains the counter ion (acetate), using an organic additive (tetrabutylammonium chloride) added to the sample and a mixture water/methanol as replacing solvent (processed just before the valve is switched to the inject position), allowed to obtain good precision of the retention time and a narrow peak for C(12)-BAK. A reversed-phase capillary based TiO(2) column and a mobile phase containing ammonium acetate at pH 5.0 for controlling the interactions of cationic surfactant with titania surface were proposed. The optimized procedure provided adequate linearity, accuracy and precision at the concentrations interval of 1.5-300 μg L(-1) .The limit of detection (LOD) was 0.5 μg L(-1) using diode array detection (DAD). The applicability of proposed IT-SPME-capillary LC method has been assessed in several water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. One-pot preparation of a mixed-mode organic-silica hybrid monolithic capillary column and its application in determination of endogenous gibberellins in plant tissues.

    Science.gov (United States)

    Zhang, Zheng; Hao, Yan-Hong; Ding, Jun; Xu, Sheng-Nan; Yuan, Bi-Feng; Feng, Yu-Qi

    2015-10-16

    A newly improved one-pot method, based on "thiol-ene" click chemistry and sol-gel approach in microemulsion system, was developed for the preparation of C8/PO(OH)2-silica hybrid monolithic capillary column. The prepared monolith possesses large specific surface area, narrow mesopore size distribution and high column efficiency. The monolithic column was demonstrated to have cation exchange/reversed-phase (CX/RP) mixed-mode retention for analytes on nano-liquid chromatography (nano-LC). On the basis of the developed nano-LC system with MS detector coupled to pipette tip solid phase extraction (PT-SPE) and derivatization process, we then realized simultaneous determination of 10 gibberellins (GAs) with low limits of detection (LODs, 0.003-0.025 ng/mL). Furthermore, 6 endogenous GAs in only 5mg rice leaves (fresh weight) were successfully detected and quantified. The developed PT-SPE-nano-LC-MS strategy may offer promising applications in the determination of low abundant bioactive molecules from complex matrix. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Selective purge for hydrogenation reactor recycle loop

    Science.gov (United States)

    Baker, Richard W.; Lokhandwala, Kaaeid A.

    2001-01-01

    Processes and apparatus for providing improved contaminant removal and hydrogen recovery in hydrogenation reactors, particularly in refineries and petrochemical plants. The improved contaminant removal is achieved by selective purging, by passing gases in the hydrogenation reactor recycle loop or purge stream across membranes selective in favor of the contaminant over hydrogen.

  2. Design and development of pressure and repressurization purge system for reusable space shuttle multilayer insulation system

    Science.gov (United States)

    1972-01-01

    The experimental determination of purge bag materials properties, development of purge bag manufacturing techniques, experimental evaluation of a subscale purge bag under simulated operating conditions and the experimental evaluation of the purge pin concept for MLI purging are discussed. The basic purge bag material, epoxy fiberglass bounded by skins of FEP Teflon, showed no significant permeability to helium flow under normal operating conditions. Purge bag small scale manufacturing tests were conducted to develop tooling and fabrication techniques for use in full scale bag manufacture. A purge bag material layup technique was developed whereby the two plys of epoxy fiberglass enclosed between skins of FEP Teflon are vacuum bag cured in an oven in a single operation. The material is cured on a tool with the shape of a purge bag half. Plastic tooling was selected for use in bag fabrication. A model purge bag 0.6 m in diameter was fabricated and subjected to a series of structural and environmental tests simulating various flight type environments. Pressure cycling tests at high (450 K) and low (200 K) temperature as well as acoustic loading tests were performed. The purge bag concept proved to be structurally sound and was used for the full scale bag detailed design model.

  3. Verification of the ASTM G-124 Purge Equation

    Science.gov (United States)

    Robbins, Katherine E.; Davis, Samuel Eddie

    2009-01-01

    ASTM G-124 seeks to evaluate combustion characteristics of metals in high-purity (greater than 99%) oxygen atmospheres. ASTM G-124 provides the following equation to determine the minimum number of purges required to reach this level of purity in a test chamber: n = -4/log10(Pa/Ph), where "n" is the total number of purge cycles required, Ph is the absolute pressure used for the purge on each cycle and Pa is the atmospheric pressure or the vent pressure. The origin of this equation is not known and has been the source of frequent questions as to its accuracy and reliability. This paper shows the derivation of the G-124 purge equation, and experimentally explores the equation to determine if it accurately predicts the number of cycles required.

  4. A Chip-Capillary Hybrid Device for Automated Transfer of Sample Pre-Separated by Capillary Isoelectric Focusing to Parallel Capillary Gel Electrophoresis for Two-Dimensional Protein Separation

    Science.gov (United States)

    Lu, Joann J.; Wang, Shili; Li, Guanbin; Wang, Wei; Pu, Qiaosheng; Liu, Shaorong

    2012-01-01

    In this report, we introduce a chip-capillary hybrid device to integrate capillary isoelectric focusing (CIEF) with parallel capillary sodium dodecyl sulfate – polyacrylamide gel electrophoresis (SDS-PAGE) or capillary gel electrophoresis (CGE) toward automating two-dimensional (2D) protein separations. The hybrid device consists of three chips that are butted together. The middle chip can be moved between two positions to re-route the fluidic paths, which enables the performance of CIEF and injection of proteins partially resolved by CIEF to CGE capillaries for parallel CGE separations in a continuous and automated fashion. Capillaries are attached to the other two chips to facilitate CIEF and CGE separations and to extend the effective lengths of CGE columns. Specifically, we illustrate the working principle of the hybrid device, develop protocols for producing and preparing the hybrid device, and demonstrate the feasibility of using this hybrid device for automated injection of CIEF-separated sample to parallel CGE for 2D protein separations. Potentials and problems associated with the hybrid device are also discussed. PMID:22830584

  5. A stochastic view on column efficiency.

    Science.gov (United States)

    Gritti, Fabrice

    2018-03-09

    A stochastic model of transcolumn eddy dispersion along packed beds was derived. It was based on the calculation of the mean travel time of a single analyte molecule from one radial position to another. The exchange mechanism between two radial positions was governed by the transverse dispersion of the analyte across the column. The radial velocity distribution was obtained by flow simulations in a focused-ion-beam scanning electron microscopy (FIB-SEM) based 3D reconstruction from a 2.1 mm × 50 mm column packed with 2 μm BEH-C 18 particles. Accordingly, the packed bed was divided into three coaxial and uniform zones: (1) a 1.4 particle diameter wide, ordered, and loose packing at the column wall (velocity u w ), (2) an intermediate 130 μm wide, random, and dense packing (velocity u i ), and (3) the bulk packing in the center of the column (velocity u c ). First, the validity of this proposed stochastic model was tested by adjusting the predicted to the observed reduced van Deemter plots of a 2.1 mm × 50 mm column packed with 2 μm BEH-C 18 fully porous particles (FPPs). An excellent agreement was found for u i  = 0.93u c , a result fully consistent with the FIB-SEM observation (u i  = 0.95u c ). Next, the model was used to measure u i  = 0.94u c for 2.1 mm × 100 mm column packed with 1.6 μm Cortecs-C 18 superficially porous particles (SPPs). The relative velocity bias across columns packed with SPPs is then barely smaller than that observed in columns packed with FPPs (+6% versus + 7%). u w =1.8u i is measured for a 75 μm × 1 m capillary column packed with 2 μm BEH-C 18 particles. Despite this large wall-to-center velocity bias (+80%), the presence of the thin and ordered wall packing layer has no negative impact on the kinetic performance of capillary columns. Finally, the stochastic model of long-range eddy dispersion explains why analytical (2.1-4.6 mm i.d.) and capillary (columns can all be

  6. Automatic and integrated micro-enzyme assay (AIμEA) platform for highly sensitive thrombin analysis via an engineered fluorescence protein-functionalized monolithic capillary column.

    Science.gov (United States)

    Lin, Lihua; Liu, Shengquan; Nie, Zhou; Chen, Yingzhuang; Lei, Chunyang; Wang, Zhen; Yin, Chao; Hu, Huiping; Huang, Yan; Yao, Shouzhuo

    2015-04-21

    Nowadays, large-scale screening for enzyme discovery, engineering, and drug discovery processes require simple, fast, and sensitive enzyme activity assay platforms with high integration and potential for high-throughput detection. Herein, a novel automatic and integrated micro-enzyme assay (AIμEA) platform was proposed based on a unique microreaction system fabricated by a engineered green fluorescence protein (GFP)-functionalized monolithic capillary column, with thrombin as an example. The recombinant GFP probe was rationally engineered to possess a His-tag and a substrate sequence of thrombin, which enable it to be immobilized on the monolith via metal affinity binding, and to be released after thrombin digestion. Combined with capillary electrophoresis-laser-induced fluorescence (CE-LIF), all the procedures, including thrombin injection, online enzymatic digestion in the microreaction system, and label-free detection of the released GFP, were integrated in a single electrophoretic process. By taking advantage of the ultrahigh loading capacity of the AIμEA platform and the CE automatic programming setup, one microreaction column was sufficient for many times digestion without replacement. The novel microreaction system showed significantly enhanced catalytic efficiency, about 30 fold higher than that of the equivalent bulk reaction. Accordingly, the AIμEA platform was highly sensitive with a limit of detection down to 1 pM of thrombin. Moreover, the AIμEA platform was robust and reliable to detect thrombin in human serum samples and its inhibition by hirudin. Hence, this AIμEA platform exhibits great potential for high-throughput analysis in future biological application, disease diagnostics, and drug screening.

  7. Acceptance/Operational Test Report for Tank 241-AN-104 camera and camera purge control system

    International Nuclear Information System (INIS)

    Castleberry, J.L.

    1995-11-01

    This Acceptance/Operational Test Procedure (ATP/OTP) will document the satisfactory operation of the camera purge panel, purge control panel, color camera system and associated control components destined for installation. The final acceptance of the complete system will be performed in the field. The purge panel and purge control panel will be tested for its safety interlock which shuts down the camera and pan-and-tilt inside the tank vapor space during loss of purge pressure and that the correct purge volume exchanges are performed as required by NFPA 496. This procedure is separated into seven sections. This Acceptance/Operational Test Report documents the successful acceptance and operability testing of the 241-AN-104 camera system and camera purge control system

  8. Colloid mobilization and transport during capillary fringe fluctuations.

    Science.gov (United States)

    Aramrak, Surachet; Flury, Markus; Harsh, James B; Zollars, Richard L

    2014-07-01

    Capillary fringe fluctuations due to changing water tables lead to displacement of air-water interfaces in soils and sediments. These moving air-water interfaces can mobilize colloids. We visualized colloids interacting with moving air-water interfaces during capillary fringe fluctuations by confocal microscopy. We simulated capillary fringe fluctuations in a glass-bead-filled column. We studied four specific conditions: (1) colloids suspended in the aqueous phase, (2) colloids attached to the glass beads in an initially wet porous medium, (3) colloids attached to the glass beads in an initially dry porous medium, and (4) colloids suspended in the aqueous phase with the presence of a static air bubble. Confocal images confirmed that the capillary fringe fluctuations affect colloid transport behavior. Hydrophilic negatively charged colloids initially suspended in the aqueous phase were deposited at the solid-water interface after a drainage passage, but then were removed by subsequent capillary fringe fluctuations. The colloids that were initially attached to the wet or dry glass bead surface were detached by moving air-water interfaces in the capillary fringe. Hydrophilic negatively charged colloids did not attach to static air-bubbles, but hydrophobic negatively charged and hydrophilic positively charged colloids did. Our results demonstrate that capillary fringe fluctuations are an effective means for colloid mobilization.

  9. Automation and integration of multiplexed on-line sample preparation with capillary electrophoresis for DNA sequencing

    Energy Technology Data Exchange (ETDEWEB)

    Tan, H.

    1999-03-31

    The purpose of this research is to develop a multiplexed sample processing system in conjunction with multiplexed capillary electrophoresis for high-throughput DNA sequencing. The concept from DNA template to called bases was first demonstrated with a manually operated single capillary system. Later, an automated microfluidic system with 8 channels based on the same principle was successfully constructed. The instrument automatically processes 8 templates through reaction, purification, denaturation, pre-concentration, injection, separation and detection in a parallel fashion. A multiplexed freeze/thaw switching principle and a distribution network were implemented to manage flow direction and sample transportation. Dye-labeled terminator cycle-sequencing reactions are performed in an 8-capillary array in a hot air thermal cycler. Subsequently, the sequencing ladders are directly loaded into a corresponding size-exclusion chromatographic column operated at {approximately} 60 C for purification. On-line denaturation and stacking injection for capillary electrophoresis is simultaneously accomplished at a cross assembly set at {approximately} 70 C. Not only the separation capillary array but also the reaction capillary array and purification columns can be regenerated after every run. DNA sequencing data from this system allow base calling up to 460 bases with accuracy of 98%.

  10. Filling of charged cylindrical capillaries

    NARCIS (Netherlands)

    Das, Siddhartha; Chanda, Sourayon; Eijkel, J.C.T.; Tas, N.R.; Chakraborty, Suman; Mitra, Sushanta K.

    2014-01-01

    We provide an analytical model to describe the filling dynamics of horizontal cylindrical capillaries having charged walls. The presence of surface charge leads to two distinct effects: It leads to a retarding electrical force on the liquid column and also causes a reduced viscous drag force because

  11. Solute transport in a well under slow-purge and no-purge conditions

    Science.gov (United States)

    Plummer, M. A.; Britt, S. L.; Martin-Hayden, J. M.

    2010-12-01

    Non-purge sampling techniques, such as diffusion bags and in-situ sealed samplers, offer reliable and cost-effective groundwater monitoring methods that are a step closer to the goal of real-time monitoring without pumping or sample collection. Non-purge methods are, however, not yet completely accepted because questions remain about how solute concentrations in an unpurged well relate to concentrations in the adjacent formation. To answer questions about how undisturbed well water samples compare to formation concentrations, and to provide the information necessary to interpret results from non-purge monitoring systems, we have conducted a variety of physical experiments and numerical simulations of flow and transport in and through monitoring wells under low-flow and ambient flow conditions. Previous studies of flow and transport in wells used a Darcy’s law - based continuity equation for flow, which is often justified under the strong, forced-convection flow caused by pumping or large vertical hydraulic potential gradients. In our study, we focus on systems with weakly forced convection, where density-driven free convection may be of similar strength. We therefore solved Darcy’s law for porous media domains and the Navier Stokes equations for flow in the well, and coupled solution of the flow equations to that of solute transport. To illustrate expected in-well transport behavior under low-flow conditions, we present results of three particular studies: (1) time-dependent effluent concentrations from a well purged at low-flow pumping rates, (2) solute-driven density effects in a well under ambient horizontal flow and (3) temperature-driven mixing in a shallow well subject to seasonal temperature variations. Results of the first study illustrate that assumptions about the nature of in-well flow have a significant impact on effluent concentration curves even during pumping, with Poiseuille-type flow producing more rapid removal of concentration differences

  12. [Determination of acetochlor and oxyfluorfen by capillary gas chromatography].

    Science.gov (United States)

    Xiang, Wen-Sheng; Wang, Xiang-Jing; Wang, Jing; Wang, Qing

    2002-09-01

    A method is described for the determination of acetochlor and oxyfluorfen by capillary gas chromatography with FID and an SE-30 capillary column (60 m x 0.53 mm i. d., 1.5 microm), using dibutyl phthalate as the internal standard. The standard deviations for acetochlor and oxyfluorfen concentration(mass fraction) were 0.44% and 0.47% respectively. The relative standard deviations for acetochlor and oxyfluorfen were 0.79% and 0.88% and the average recoveries for acetochlor and oxyfluorfen were 99.3% and 101.1% respectively. The method is simple, rapid and accurate.

  13. Realization of dynamic data migration and purge operations

    International Nuclear Information System (INIS)

    Wang Juan; Qiu Hongmao; Liu Junmin; Wang Xiaoming; Wang Hong; Zhong Bo; Lu Yuanlei; Xu Jin

    2008-01-01

    In the large scale real time data processing, with the time extend, the data in database system will be expanded, which declines the system capability. To solve the problem, this paper presents a method of migration and purge operations. New or updated database records within a specified time interval can be copied automatically from source database accounts to destination database accounts and the data in the source database will be deleted automatically after a specified period of time according to the rules using the method. The migration and purge operations have been realized in China National Data Center. (authors)

  14. Technical Note: A fully automated purge and trap GC-MS system for quantification of volatile organic compound (VOC fluxes between the ocean and atmosphere

    Directory of Open Access Journals (Sweden)

    S. J. Andrews

    2015-04-01

    Full Text Available The oceans are a key source of a number of atmospherically important volatile gases. The accurate and robust determination of trace gases in seawater is a significant analytical challenge, requiring reproducible and ideally automated sample handling, a high efficiency of seawater–air transfer, removal of water vapour from the sample stream, and high sensitivity and selectivity of the analysis. Here we describe a system that was developed for the fully automated analysis of dissolved very short-lived halogenated species (VSLS sampled from an under-way seawater supply. The system can also be used for semi-automated batch sampling from Niskin bottles filled during CTD (conductivity, temperature, depth profiles. The essential components comprise a bespoke, automated purge and trap (AutoP & T unit coupled to a commercial thermal desorption and gas chromatograph mass spectrometer (TD-GC-MS. The AutoP & T system has completed five research cruises, from the tropics to the poles, and collected over 2500 oceanic samples to date. It is able to quantify >25 species over a boiling point range of 34–180 °C with Henry's law coefficients of 0.018 and greater (CH22l, kHcc dimensionless gas/aqueous and has been used to measure organic sulfurs, hydrocarbons, halocarbons and terpenes. In the eastern tropical Pacific, the high sensitivity and sampling frequency provided new information regarding the distribution of VSLS, including novel measurements of a photolytically driven diurnal cycle of CH22l within the surface ocean water.

  15. Distinguishing Between Risk Factors for Bulimia Nervosa, Binge Eating Disorder, and Purging Disorder.

    Science.gov (United States)

    Allen, Karina L; Byrne, Susan M; Crosby, Ross D

    2015-08-01

    Binge eating disorder and purging disorder have gained recognition as distinct eating disorder diagnoses, but risk factors for these conditions have not yet been established. This study aimed to evaluate a prospective, mediational model of risk for the full range of binge eating and purging eating disorders, with attention to possible diagnostic differences. Specific aims were to determine, first, whether eating, weight and shape concerns at age 14 would mediate the relationship between parent-perceived childhood overweight at age 10 and a binge eating or purging eating disorder between age 15 and 20, and, second, whether this mediational model would differ across bulimia nervosa, binge eating disorder, and purging disorder. Participants (N = 1,160; 51 % female) were drawn from the Western Australian Pregnancy Cohort (Raine) Study, which has followed children from pre-birth to age 20. Eating disorders were assessed via self-report questionnaires when participants were aged 14, 17 and 20. There were 146 participants (82 % female) with a binge eating or purging eating disorder with onset between age 15 and 20 [bulimia nervosa = 81 (86 % female), binge eating disorder = 43 (74 % female), purging disorder = 22 (77 % female)]. Simple mediation analysis with bootstrapping was used to test the hypothesized model of risk, with early adolescent eating, weight and shape concerns positioned as a mediator between parent-perceived childhood overweight and later onset of a binge eating or purging eating disorder. Subsequently, a conditional process model (a moderated mediation model) was specified to determine if model pathways differed significantly by eating disorder diagnosis. In the simple mediation model, there was a significant indirect effect of parent-perceived childhood overweight on risk for a binge eating or purging eating disorder in late adolescence, mediated by eating, weight and shape concerns in early adolescence. In the conditional process model

  16. Capillary pressure and saturation relations for supercritical CO2 and brine in sand: High-pressure Pc(Sw) controller/meter measurements and capillary scaling predictions

    Science.gov (United States)

    Tokunaga, Tetsu K.; Wan, Jiamin; Jung, Jong-Won; Kim, Tae Wook; Kim, Yongman; Dong, Wenming

    2013-08-01

    In geologic carbon sequestration, reliable predictions of CO2 storage require understanding the capillary behavior of supercritical (sc) CO2. Given the limited availability of measurements of the capillary pressure (Pc) dependence on water saturation (Sw) with scCO2 as the displacing fluid, simulations of CO2 sequestration commonly rely on modifying more familiar air/H2O and oil/H2O Pc(Sw) relations, adjusted to account for differences in interfacial tensions. In order to test such capillary scaling-based predictions, we developed a high-pressure Pc(Sw) controller/meter, allowing accurate Pc and Sw measurements. Drainage and imbibition processes were measured on quartz sand with scCO2-brine at pressures of 8.5 and 12.0 MPa (45°C), and air-brine at 21°C and 0.1 MPa. Drainage and rewetting at intermediate Sw levels shifted to Pc values that were from 30% to 90% lower than predicted based on interfacial tension changes. Augmenting interfacial tension-based predictions with differences in independently measured contact angles from different sources led to more similar scaled Pc(Sw) relations but still did not converge onto universal drainage and imbibition curves. Equilibrium capillary trapping of the nonwetting phases was determined for Pc = 0 during rewetting. The capillary-trapped volumes for scCO2 were significantly greater than for air. Given that the experiments were all conducted on a system with well-defined pore geometry (homogeneous sand), and that scCO2-brine interfacial tensions are fairly well constrained, we conclude that the observed deviations from scaling predictions resulted from scCO2-induced decreased wettability. Wettability alteration by scCO2 makes predicting hydraulic behavior more challenging than for less reactive fluids.

  17. One column method to prepare 11C-labelled methyl iodide

    International Nuclear Information System (INIS)

    Kovacs, Z.; Priboczki, E.

    1999-01-01

    A new method in which the [ 11 C]methyl iodide is prepared on one alumina column is presented. A high specific surface alumina column, previously impregnated with lithium aluminium hydride solution, was used for direct trapping from the target gas and reduction into radiocomplex. The complex was then reacted on this column with HI to form [ 11 C]methyl iodide. The use of one alumina column, instead of a freezing trap, reaction vessel and separate unit for iodination, simplifies the apparatus, shortens the synthesis time and is well suitable for automation. (K.A.)

  18. Modeling aerobic biodegradation in the capillary fringe.

    Science.gov (United States)

    Luo, Jian; Kurt, Zohre; Hou, Deyi; Spain, Jim C

    2015-02-03

    Vapor intrusion from volatile subsurface contaminants can be mitigated by aerobic biodegradation. Laboratory column studies with contaminant sources of chlorobenzene and a mixture of chlorobenzene, 1,2-dichlorobenzene, and 1,4-dichlorobenzene showed that contaminants were rapidly degraded in thin reactive zones with high biomass and low substrate concentrations in the vicinity of the capillary fringe. Such behavior was well characterized by a model that includes oxygen-, substrate-, and biomass-dependent biodegradation kinetics along with diffusive transport processes. An analytical solution was derived to provide theoretical support for the simplification of reaction kinetics and the approximation of reactive zone location and mass flux relationships at steady state. Results demonstrate the potential of aerobic natural attenuation in the capillary fringe for preventing contaminant migration in the unsaturated zone. The solution indicates that increasing contaminant mass flux into the column creates a thinner reactive zone and pushes it toward the oxygen boundary, resulting in a shorter distance to the oxygen source and a larger oxygen mass flux that balances the contaminant mass flux. As a consequence, the aerobic biodegradation can reduce high contaminant concentrations to low levels within the capillary fringe and unsaturated zone. The results are consistent with the observations of thin reactive layers at the interface in unsaturated zones. The model considers biomass while including biodegradation in the capillary fringe and unsaturated zone and clearly demonstrates that microbial communities capable of using the contaminants as electron donors may lead to instantaneous degradation kinetics in the capillary fringe and unsaturated zone.

  19. Multi-Capillary Column-Ion Mobility Spectrometry of Volatile Metabolites Emitted by Saccharomyces Cerevisiae

    Directory of Open Access Journals (Sweden)

    Christoph Halbfeld

    2014-09-01

    Full Text Available Volatile organic compounds (VOCs produced during microbial fermentations determine the flavor of fermented food and are of interest for the production of fragrances or food additives. However, the microbial synthesis of these compounds from simple carbon sources has not been well investigated so far. Here, we analyzed the headspace over glucose minimal salt medium cultures of Saccharomyces cerevisiae using multi-capillary column-ion mobility spectrometry (MCC-IMS. The high sensitivity and fast data acquisition of the MCC-IMS enabled online analysis of the fermentation off-gas and 19 specific signals were determined. To four of these volatile compounds, we could assign the metabolites ethanol, 2-pentanone, isobutyric acid, and 2,3-hexanedione by MCC-IMS measurements of pure standards and cross validation with thermal desorption–gas chromatography-mass spectrometry measurements. Despite the huge biochemical knowledge of the biochemistry of the model organism S. cerevisiae, only the biosynthetic pathways for ethanol and isobutyric acid are fully understood, demonstrating the considerable lack of research of volatile metabolites. As monitoring of VOCs produced during microbial fermentations can give valuable insight into the metabolic state of the organism, fast and non-invasive MCC-IMS analyses provide valuable data for process control.

  20. A fast and accurate method for the pharmacokinetic research of four coumarin analogs in Fructus cnidii using capillary electro-chromatography with a methacrylate ester-based monolithic column.

    Science.gov (United States)

    Chen, Zhao; Xu, Aili; Bi, Xiaoli; Luo, Wenhui; Li, Ji; Fan, Guorong; Sun, Dongmei

    2017-11-01

    In the present study, a monolithic capillary column with higher permeability was developed for the in vivo discrimination of four coumarin analogs (bergapten, 2'-acetylangelicin, imperatorin, and osthole) that typically require long separation times in HPLC. Instead of conventional methacrylate ester monolith (containing 19.5% porogen) with insufficient permeability (K = 1.52 - 1.66 × 10 -14 M 2 ) for plasma sample, the proposed column (20.5% porogen) had better permeability (around 3.80 × 10 -14 M 2 ) while properties such as pore distribution, stability, and resolution changed slightly. As a result, due to the negatively charged electro-dynamic flow of the methacrylate ester groups in the monolith, the migration of targeted analytes was achieved within 6 min (compared with 30 min in HPLC) with acceptable resolution and improved sensitivity (0.005-0.02 μg/mL vs. 0.04 μg/mL). The proposed method was also applied to pharmacokinetic research: accelerated solvent extraction (ASE) was used to improve the extraction efficiency, which prepared extract much faster and more pure than conventional methods. As the pharmacokinetic parameters indicated, the monolithic capillary electro-chromatography method was efficient, sensitive, specific, and durable, guaranteeing its utility for the determination of multiple structure-related compounds in rat plasma. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Characterization of polymer monolithic stationary phases for capillary HPLC

    Czech Academy of Sciences Publication Activity Database

    Moravcová, D.; Jandera, P.; Urban, J.; Planeta, Josef

    2003-01-01

    Roč. 26, č. 11 (2003), s. 1005-1016 ISSN 1615-9306 R&D Projects: GA ČR GA203/02/0023 Institutional research plan: CEZ:AV0Z4031919; CEZ:MSM 253100002 Keywords : monolithic column s * capillary HPLC * column testing Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.108, year: 2003

  2. Use of experimental design for the purge-and-trap-gas chromatography-mass spectrometry determination of methyl tert.-butyl ether, tert.-butyl alcohol and BTEX in groundwater at trace level.

    Science.gov (United States)

    Bianchi, F; Careri, M; Marengo, E; Musci, M

    2002-10-25

    An efficient method for the simultaneous determination of methyl tert.-butyl ether, tert.-butyl alcohol, benzene, toluene, ethylbenzene and xylene isomers in groundwater by purge-and-trap-gas chromatography-mass spectrometry was developed and validated. Experimental design was used to investigate the effects of temperature of extraction, time of extraction and percentage of salt added to the water samples. Regression models and desirability functions were applied to find the experimental conditions providing the highest global extraction yield. Validation was carried out in terms of limits of detection (LOD), limits of quantitation (LOQ), linearity and precision. LOD values ranging from 2.6 to 23 ng l(-1) were achieved, whereas linearity was statistically verified over two orders of magnitude for each compound. Precision was evaluated testing two concentration levels. Good results were obtained both in terms of intra-day repeatability and intermediate precision: RSD% lower than 4.5% at the highest concentration and lower than 13% at the lowest one were calculated for intra-day repeatability. A groundwater sample suspected of contamination by leaking underground petroleum storage tanks was analysed and some of the analytes were detected and quantitated.

  3. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

    1996-01-01

    A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

  4. Preparation and evaluation of 400μm I.D. polymer-based hydrophilic interaction chromatography monolithic columns with high column efficiency.

    Science.gov (United States)

    Liu, Chusheng; Li, Haibin; Wang, Qiqin; Crommen, Jacques; Zhou, Haibo; Jiang, Zhengjin

    2017-08-04

    The quest for higher column efficiency is one of the major research areas in polymer-based monolithic column fabrication. In this research, two novel polymer-based HILIC monolithic columns with 400μm I.D.×800μm O.D. were prepared based on the thermally initiated co-polymerization of N,N-dimethyl-N-(3-methacrylamidopropyl)-N-(3-sulfopropyl) ammonium betaine (SPP) and ethylene glycol dimethacrylate (EDMA) or N,N'-methylenebisacrylamide (MBA). In order to obtain a satisfactory performance in terms of column permeability, mechanical stability, efficiency and selectivity, the polymerization parameters were systematically optimized. Column efficiencies as high as 142, 000 plates/m and 120, 000 plates/m were observed for the analysis of neutral compounds at 0.6mm/s on the poly(SPP-co-MBA) and poly(SPP-co-EDMA) monoliths, respectively. Furthermore, the Van Deemter plots for thiourea on the two monoliths were compared with that on a commercial silica based ZIC-HILIC column (3.5μm, 200Å, 150mm×300μm I.D.) using ACN/H 2 O (90/10, v/v) as the mobile phase at room temperature. It was noticeable that the Van Deemter curves for both monoliths, particularly the poly(SPP-co-MBA) monolith, are significantly flatter than that obtained for the ZIC-HILIC column, which indicates that in spite of their larger internal diameters, they yield better overall efficiency, with less peak dispersion, across a much wider range of usable linear velocities. A clearly better separation performance was also observed for nucleobases, nucleosides, nucleotides and small peptides on the poly(SPP-co-MBA) monolith compared to the ZIC-HILIC column. It is particularly worth mentioning that these 400μm I.D. polymer-based HILIC monolithic columns exhibit enhanced mechanical strength owing to the thicker capillary wall of the fused-silica capillaries. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Acoustic trapping in bubble-bounded micro-cavities

    Science.gov (United States)

    O'Mahoney, P.; McDougall, C.; Glynne-Jones, P.; MacDonald, M. P.

    2016-12-01

    We present a method for controllably producing longitudinal acoustic trapping sites inside microfluidic channels. Air bubbles are injected into a micro-capillary to create bubble-bounded `micro-cavities'. A cavity mode is formed that shows controlled longitudinal acoustic trapping between the two air/water interfaces along with the levitation to the centre of the channel that one would expect from a lower order lateral mode. 7 μm and 10 μm microspheres are trapped at the discrete acoustic trapping sites in these micro-cavities.We show this for several lengths of micro-cavity.

  6. Simultaneous separation of water- and fat-soluble vitamins in isocratic pressure-assisted capillary electrochromatography using a methacrylate-based monolithic column.

    Science.gov (United States)

    Yamada, Hiroki; Kitagawa, Shinya; Ohtani, Hajime

    2013-06-01

    A method of simultaneous separation of water- and fat-soluble vitamins using pressure-assisted CEC with a methacrylate-based capillary monolithic column was developed. In the proposed method, water-soluble vitamins were mainly separated electrophoretically, while fat soluble-ones were separated chromatographically by the interaction with a methacrylate-based monolith. A mixture of six water-soluble and four fat-soluble vitamins was separated simultaneously within 20 min with an isocratic elution using 1 M formic acid (pH 1.9)/acetonitrile (30:70, v/v) containing 10 mM ammonium formate as a mobile phase. When the method was applied to a commercial multivitamin tablet and a spiked one, the vitamins were successfully analyzed, and no influence of the matrix contained in the tablet was observed. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Multi-column adsorption systems with condenser for tritiated water vapor removal

    International Nuclear Information System (INIS)

    Kotoh, Kenji; Kudo, Kazuhiko

    1996-01-01

    Two types of multi-column adsorption system are proposed as the system for removal of tritiated moisture from tritium process gases or/and handling room atmospheres. The types are of recycle use of adsorption columns, and are composed of twin or triplet columns and one condenser which is used for collecting the adsorbed moisture from columns in desorption process. The systems utilize the dry gas from a working column as the purge gas for regenerating a saturated column and appropriate an active column for recovery of the tritiated moisture passing through the condenser. Each column hence needs the additional amount of adsorbent for collecting the moisture from the condenser. In the modeling and design of an adsorption column, it is primary to estimate the necessary amount of a candidate adsorbent for its packed-bed. The performance of the proposed systems is examined here by analyzing the dependence of the necessary amount of adsorbent for their columns on process operational conditions and adsorbent moisture-adsorption characteristics. The result shows that the necessary amount is sensitive to the types of adsorption isotherm, and suggests that these systems should employ adsorbents which exhibit the Langmuir-type isotherms. (author)

  8. π-Extended triptycene-based material for capillary gas chromatographic separations.

    Science.gov (United States)

    Yang, Yinhui; Wang, Qinsi; Qi, Meiling; Huang, Xuebin

    2017-10-02

    Triptycene-based materials feature favorable physicochemical properties and unique molecular recognition ability that offer good potential as stationary phases for capillary gas chromatography (GC). Herein, we report the investigation of utilizing a π-extended triptycene material (denoted as TQPP) for GC separations. As a result, the TQPP capillary column exhibited high column efficiency of 4030 plates m -1 and high-resolution performance for a wide range of analytes, especially structural and positional isomers. Interestingly, the TQPP stationary phase showed unique shape selectivity for alkanes isomers and preferential retention for analytes with halogen atoms and H-bonding nature mainly through their halogen-bonding and H-bonding interactions. In addition, the TQPP column had good repeatability and reproducibility with the RSD values of 0.02-0.34% for run-to-run, 0.09-0.80% for day-to-day and 1.4-5.2% for column-to-column, respectively, and favorable thermal stability up to 280 °C. This work demonstrates the promising future of triptycene-based materials as a new class of stationary phases for GC separations. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Capillary electrophoretic separation of inorganic and organic arsenic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Greschonig, H. [Institute of Analytical Chemistry, Karl Franzens University Graz (Austria); Schmid, M.G.; Guebitz, G. [Institute of Pharmaceutical Chemistry, Karl Franzens University Graz (Austria)

    1998-09-01

    Capillary zone electrophoresis was used to separate arsenite, arsenate, dimethylarsinic and diphenylarsinic acid, methanearsonic acid, phenyl- and p-aminophenyl arsonic acid, phenylarsineoxide and phenarsazinic acid. Anionic and uncharged species were separated in a fused silica capillary with on-column UV detection at 200 nm. A 15 mM phosphate solution adjusted to pH 6.5 containing 10 mM sodium dodecylsulfonate served as background electrolyte. The influence of pH and applied voltage on separation efficiency, as well as the feasibility of identification of arsenic compounds in spiked urine, were investigated. (orig.) With 7 figs., 1 tab., 22 refs.

  10. New capillary number definition for displacement of residual nonwetting phase in natural fractures

    NARCIS (Netherlands)

    Alquaimi, B.; Rossen, W.R.

    2017-01-01

    We propose a new capillary number for flow in fractures starting with a force balance on a trapped ganglion in a fracture. The new definition is validated with laboratory experiments using five distinctive model fractures. Capillary desaturation curves were generated experimentally using

  11. Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong

    2013-07-01

    A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Numerical analysis of capillary entrapment for effective CO{sub 2} aquifer storage

    Energy Technology Data Exchange (ETDEWEB)

    Uelker, B.; Pusch, G. [Technische Univ. Clausthal (Germany). Inst. fuer Erdoel- und Erdgastechnik; May, F. [Bundesanstalt fuer Geowissenschaften und Rohstoffe, Hannover (Germany)

    2007-09-13

    The success of underground CO{sub 2} sequestration projects relies on the ability of keeping CO{sub 2} immobilized. The risk of CO{sub 2} leakage into the atmosphere through faults, cap rock formations or wellbore must be evaluated for the long term safety of storage. In case of CO{sub 2} sequestration in a saline aquifer capillary trapping of CO{sub 2} is one of the essential mechanisms controlling the upward and lateral migration of CO{sub 2} plumes after the injection phase. Therefore, assessment of CO{sub 2} immobilization requires accurate modelling of multi phase flow performance. A generic reservoir model was created to examine the impact of the relative permeabilities and capillary forces on capillary trapping. This study reveals how the mechanism of capillary trapping is affected by varying the CO{sub 2} injection rate, hysteresis between drainage and imbibition processes and residual phase saturations. The leakage risk of injected CO{sub 2} in vertical and horizontal wells was also compared to identify the effective injection geometry. Vertical injection across the entire storage formation interval leads to extensive contact with cap rock and leakage through it. Horizontal wells located in the lower part of the formation both increase the aquifer utilization and eliminate contact with cap rock immediately. Thus horizontal wells can be an alternative to inject more CO{sub 2} and minimize leakage. (orig.)

  13. ATR/OTR-SY Tank Camera Purge System and in Tank Color Video Imaging System

    International Nuclear Information System (INIS)

    Werry, S.M.

    1995-01-01

    This procedure will document the satisfactory operation of the 101-SY tank Camera Purge System (CPS) and 101-SY in tank Color Camera Video Imaging System (CCVIS). Included in the CPRS is the nitrogen purging system safety interlock which shuts down all the color video imaging system electronics within the 101-SY tank vapor space during loss of nitrogen purge pressure

  14. The hummingbird tongue is a fluid trap, not a capillary tube

    OpenAIRE

    Rico-Guevara, Alejandro; Rubega, Margaret A.

    2011-01-01

    Hummingbird tongues pick up a liquid, calorie-dense food that cannot be grasped, a physical challenge that has long inspired the study of nectar-transport mechanics. Existing biophysical models predict optimal hummingbird foraging on the basis of equations that assume that fluid rises through the tongue in the same way as through capillary tubes. We demonstrate that the hummingbird tongue does not function like a pair of tiny, static tubes drawing up floral nectar via capillary action. Instea...

  15. Surfing with capillary waves: a survival strategy for trapped bees

    Science.gov (United States)

    Roh, Chris; Gharib, Morteza

    2017-11-01

    Honeybees are able to propel themselves at the water surface. A rapid vibration (30-220 Hz) of wings at the air-water interface results in a locomotion speed of 3-4 cm/s. A mechanism for generating thrust required for achieving and maintaining such speed must be different from their mechanism of flight inasmuch as they are in a different fluid environment. In this study, we present the thrust generating mechanism of the honeybee at the air-water interface. A close observation of the wing's interaction with the water surface showed that the wing does not penetrate nor detach from the water surface. Moreover, the stroke speed of the wing exceeds the minimum capillary wave speed, which signifies that the wing constantly generates the capillary wave by pulling on the surface with its wetted underside. Observation of such interaction suggests that honeybee's locomotion at the water surface resembles surfing on the self-generated capillary wave. A further evidence of described mechanism is explored by constructing a similarly sized mechanical model. This material is based upon work supported by the National Science Foundation under Grant No. CBET-1511414; additional support by the National Science Foundation Graduate Research Fellowship under Grant No. DGE-1144469.

  16. Acceptance/operational test procedure 101-AW tank camera purge system and 101-AW video camera system

    International Nuclear Information System (INIS)

    Castleberry, J.L.

    1994-01-01

    This procedure will document the satisfactory operation of the 101-AW Tank Camera Purge System (CPS) and the 101-AW Video Camera System. The safety interlock which shuts down all the electronics inside the 101-AW vapor space, during loss of purge pressure, will be in place and tested to ensure reliable performance. This procedure is separated into four sections. Section 6.1 is performed in the 306 building prior to delivery to the 200 East Tank Farms and involves leak checking all fittings on the 101-AW Purge Panel for leakage using a Snoop solution and resolving the leakage. Section 7.1 verifies that PR-1, the regulator which maintains a positive pressure within the volume (cameras and pneumatic lines), is properly set. In addition the green light (PRESSURIZED) (located on the Purge Control Panel) is verified to turn on above 10 in. w.g. and after the time delay (TDR) has timed out. Section 7.2 verifies that the purge cycle functions properly, the red light (PURGE ON) comes on, and that the correct flowrate is obtained to meet the requirements of the National Fire Protection Association. Section 7.3 verifies that the pan and tilt, camera, associated controls and components operate correctly. This section also verifies that the safety interlock system operates correctly during loss of purge pressure. During the loss of purge operation the illumination of the amber light (PURGE FAILED) will be verified

  17. Capillary gel electrophoresis for rapid, high resolution DNA sequencing.

    OpenAIRE

    Swerdlow, H; Gesteland, R

    1990-01-01

    Capillary gel electrophoresis has been demonstrated for the separation and detection of DNA sequencing samples. Enzymatic dideoxy nucleotide chain termination was employed, using fluorescently tagged oligonucleotide primers and laser based on-column detection (limit of detection is 6,000 molecules per peak). Capillary gel separations were shown to be three times faster, with better resolution (2.4 x), and higher separation efficiency (5.4 x) than a conventional automated slab gel DNA sequenci...

  18. Analysis of polycyclic aromatic hydrocarbons I. Determination by gas chromatography with glass and fused silica capillary columns; Analisis de Hidrocarburos aromaticos policiclicos. I. Determinacion por cromatografia de gases con columnas capilares de vidrio de silice fundida

    Energy Technology Data Exchange (ETDEWEB)

    Perez, M M; Gonzalez, D

    1987-07-01

    A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons is presented. The separation has been carried out by glass and fused silica capillary column. The limitations and the advantages of the procedure are discussed in terms of separation efficiency, sensitivity and precision. (Author) 17 refs.

  19. Steroids in porcine follicular fluid: analysis by HPLC, capillary CG and capillary CG/MS after purification on SEP-PAK C18 and ion exchange chromatography.

    Science.gov (United States)

    Khalil, M W; Lawson, V

    1983-04-01

    Steroids in porcine follicular fluid have been concentrated by reverse phase chromatography in SEP-PAK C18 and purified further on the cation exchanger SP-Sephadex C-25. Fractionation into unconjugated neutral and phenolic steroids, glucuronides and sulfates was carried out on triethylaminohydroxypropyl Sephadex LH-20 (TEAP-LH-20). The unconjugated neutral fraction was analysed by high pressure liquid chromatography (HPLC) on a C18 radial cartridge 5 mm I.D.; 10 mu, or on a C18 5 mu RESOLVE column, and by capillary gas chromatography (GC) on a 12 M OV-1 cross linked fused silica column. Testosterone, progesterone and androstenedione were the major steroids detected by HPLC monitored at 254 nm, although 17- hydroxy-, 20 alpha-dihydro- and 20 beta-dihydroprogesterone were also present. Pregnenolone, pregnanediol, dehydroepiandrosterone, 17-hydroxypregnenolone and androsterone were detected by capillary CG as their 0-methyloxime trimethylsilyether derivatives. Further confirmation of structure was provided by complete mass spectral data or by selective ion monitoring (SIM).

  20. Monitoring Tumour Cell Purge by Long Term Marrow Culture in Acute Leukemia

    International Nuclear Information System (INIS)

    El-Masry, M.; Hashem, T. M.

    2001-01-01

    Purging of leukemic cells from bone marrow harvested for autologous bone marrow transplantation (ABMT) remains a challenge. This work aimed at evaluating the efficacy of long-term marrow culture (LTMC) on purging leukemic progenitors in acute leukemia. Design and methods: We planned to study the presence of immunoglobulin heavy (lgH) chain gene rearrangements by polymerase chain reaction (PCR) at diagnosis for bone marrow of 23 patients with acute leukemia. LTMC was performed only for patients who showed positive IgH chain gene monoclonality at diagnosis. The efficiency of purge was evaluated by PCR for monoclonal IgH chain gene on weekly basis of LTMC. Results: Of the 23 studied cases, 18 (78.26%) showed positive clonal IgH chain gene at diagnosis. LTMC study showed that 6/]8 (33.33%), 3/18 (16.67%),7/18 (38.89%) and 2/18 (11.11 %) underwent complete purging of the leukemic progenitors at the first, second, third and fourth weeks of culture, respectively. Follow up could be performed for 14 positive ALL cases after induction of remission; 12/14 (85.7%) showed minimal residual disease (MRD) while only two cases did not show MRD. Complete purging of the latter two cases by LTMC occurred on the second and third weeks of culture. Conclusion: LTMC is a useful and successful method for leukemic cell purging. LTMC should be undertaken at initial diagnosis and on an individual basis. Each case should be dealt with solely to determine at which week of culture complete purging could be obtained for subsequent autologous grafting of the purged marrow

  1. Rugged Large Volume Injection for Sensitive Capillary LC-MS Environmental Monitoring

    Directory of Open Access Journals (Sweden)

    Hanne Roberg-Larsen

    2017-08-01

    Full Text Available A rugged and high throughput capillary column (cLC LC-MS switching platform using large volume injection and on-line automatic filtration and filter back-flush (AFFL solid phase extraction (SPE for analysis of environmental water samples with minimal sample preparation is presented. Although narrow columns and on-line sample preparation are used in the platform, high ruggedness is achieved e.g., injection of 100 non-filtrated water samples did not result in a pressure rise/clogging of the SPE/capillary columns (inner diameter 300 μm. In addition, satisfactory retention time stability and chromatographic resolution were also features of the system. The potential of the platform for environmental water samples was demonstrated with various pharmaceutical products, which had detection limits (LOD in the 0.05–12.5 ng/L range. Between-day and within-day repeatability of selected analytes were <20% RSD.

  2. Towards point of care testing for C. difficile infection by volatile profiling, using the combination of a short multi-capillary gas chromatography column with metal oxide sensor detection

    International Nuclear Information System (INIS)

    McGuire, N D; Ewen, R J; De Lacy Costello, B; Garner, C E; Vaughan, K; Ratcliffe, N M; Probert, C S J

    2014-01-01

    Rapid volatile profiling of stool sample headspace was achieved using a combination of short multi-capillary chromatography column (SMCC), highly sensitive heated metal oxide semiconductor sensor and artificial neural network software. For direct analysis of biological samples this prototype offers alternatives to conventional gas chromatography (GC) detectors and electronic nose technology. The performance was compared to an identical instrument incorporating a long single capillary column (LSCC). The ability of the prototypes to separate complex mixtures was assessed using gas standards and homogenized in house ‘standard’ stool samples, with both capable of detecting more than 24 peaks per sample. The elution time was considerably faster with the SMCC resulting in a run time of 10 min compared to 30 min for the LSCC. The diagnostic potential of the prototypes was assessed using 50 C. difficile positive and 50 negative samples. The prototypes demonstrated similar capability of discriminating between positive and negative samples with sensitivity and specificity of 85% and 80% respectively. C. difficile is an important cause of hospital acquired diarrhoea, with significant morbidity and mortality around the world. A device capable of rapidly diagnosing the disease at the point of care would reduce cases, deaths and financial burden. (paper)

  3. An Integrated Capillary, Buoyancy, and Viscous-Driven Model for Brine/CO2Relative Permeability in a Compositional and Parallel Reservoir Simulator

    KAUST Repository

    Kong, X.; Delshad, M.; Wheeler, M. F.

    2012-01-01

    The effectiveness of CO2 storage in the saline aquifers is governed by the interplay of capillary, viscous, and buoyancy forces. Recent experimental study reveals the impact of pressure, temperature, and salinity on interfacial tension (IFT) between CO2 and brine. The dependence of CO2-brine relative permeability and capillary pressure on pressure (IFT) is also clearly evident in published experimental results. Improved understanding of the mechanisms that control the migration and trapping of CO2 in subsurface is crucial to design future storage projects that warrant long-term and safe containment. Simulation studies ignoring the buoyancy and also variation in interfacial tension and the effect on the petrophysical properties such as trapped CO2 saturations, relative permeability, and capillary pressure have a poor chance of making accurate predictions of CO2 injectivity and plume migration. We have developed and implemented a general relative permeability model that combines effects of pressure gradient, buoyancy, and IFT in an equation of state (EOS) compositional and parallel simulator. The significance of IFT variations on CO2 migration and trapping is assessed.

  4. An Integrated Capillary, Buoyancy, and Viscous-Driven Model for Brine/CO2Relative Permeability in a Compositional and Parallel Reservoir Simulator

    KAUST Repository

    Kong, X.

    2012-11-03

    The effectiveness of CO2 storage in the saline aquifers is governed by the interplay of capillary, viscous, and buoyancy forces. Recent experimental study reveals the impact of pressure, temperature, and salinity on interfacial tension (IFT) between CO2 and brine. The dependence of CO2-brine relative permeability and capillary pressure on pressure (IFT) is also clearly evident in published experimental results. Improved understanding of the mechanisms that control the migration and trapping of CO2 in subsurface is crucial to design future storage projects that warrant long-term and safe containment. Simulation studies ignoring the buoyancy and also variation in interfacial tension and the effect on the petrophysical properties such as trapped CO2 saturations, relative permeability, and capillary pressure have a poor chance of making accurate predictions of CO2 injectivity and plume migration. We have developed and implemented a general relative permeability model that combines effects of pressure gradient, buoyancy, and IFT in an equation of state (EOS) compositional and parallel simulator. The significance of IFT variations on CO2 migration and trapping is assessed.

  5. Method of controlling weld chamber purge and cover gas atmosphere

    International Nuclear Information System (INIS)

    Yeo, D.

    1992-01-01

    A method of controlling the gas atmosphere in a welding chamber includes detecting the absence of a fuel rod from the welding chamber and, in response thereto, initiating the supplying of a flow of argon gas to the chamber to purge air therefrom. Further, the method includes detecting the entry of a fuel rod in the welding chamber and, in response thereto, terminating the supplying of the flow of argon gas to the chamber and initiating the supplying of a flow of helium gas to the chamber to purge argon gas therefrom and displace the argon gas in the chamber. Also, the method includes detecting the withdrawal of the fuel rod from the welding chamber and, in response thereto, terminating the supplying of the flow of helium gas to the chamber and initiating the supplying of argon to the chamber to purge the air therefrom. The method also includes detecting the initiation of a weld cycle and, in response thereto, momentarily supplying a flow of argon gas to the welding electrode tip for initiating the welding arc. (Author)

  6. Application of Homochiral Alkylated Organic Cages as Chiral Stationary Phases for Molecular Separations by Capillary Gas Chromatography.

    Science.gov (United States)

    Xie, Shengming; Zhang, Junhui; Fu, Nan; Wang, Bangjin; Hu, Cong; Yuan, Liming

    2016-11-08

    Molecular organic cage compounds have attracted considerable attention due to their potential applications in gas storage, catalysis, chemical sensing, molecular separations, etc. In this study, a homochiral pentyl cage compound was synthesized from a condensation reaction of ( S , S )-1,2-pentyl-1,2-diaminoethane and 1,3,5-triformylbenzene. The imine-linked pentyl cage diluted with a polysiloxane (OV-1701) was explored as a novel stationary phase for high-resolution gas chromatographic separation of organic compounds. Some positional isomers were baseline separated on the pentyl cage-coated capillary column. In particular, various types of enantiomers including chiral alcohols, esters, ethers and epoxides can be resolved without derivatization on the pentyl cage-coated capillary column. The reproducibility of the pentyl cage-coated capillary column for separation was investigated using nitrochlorobenzene and styrene oxide as analytes. The results indicate that the column has good stability and separation reproducibility after being repeatedly used. This work demonstrates that molecular organic cage compounds could become a novel class of chiral separation media in the near future.

  7. Application of Homochiral Alkylated Organic Cages as Chiral Stationary Phases for Molecular Separations by Capillary Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Shengming Xie

    2016-11-01

    Full Text Available Molecular organic cage compounds have attracted considerable attention due to their potential applications in gas storage, catalysis, chemical sensing, molecular separations, etc. In this study, a homochiral pentyl cage compound was synthesized from a condensation reaction of (S,S-1,2-pentyl-1,2-diaminoethane and 1,3,5-triformylbenzene. The imine-linked pentyl cage diluted with a polysiloxane (OV-1701 was explored as a novel stationary phase for high-resolution gas chromatographic separation of organic compounds. Some positional isomers were baseline separated on the pentyl cage-coated capillary column. In particular, various types of enantiomers including chiral alcohols, esters, ethers and epoxides can be resolved without derivatization on the pentyl cage-coated capillary column. The reproducibility of the pentyl cage-coated capillary column for separation was investigated using nitrochlorobenzene and styrene oxide as analytes. The results indicate that the column has good stability and separation reproducibility after being repeatedly used. This work demonstrates that molecular organic cage compounds could become a novel class of chiral separation media in the near future.

  8. Sexual Orientation Disparities in Purging and Binge Eating From Early to Late Adolescence

    Science.gov (United States)

    Austin, S. Bryn; Ziyadeh, Najat J.; Corliss, Heather L.; Rosario, Margaret; Wypij, David; Haines, Jess; Camargo, Carlos A.; Field, Alison E.

    2009-01-01

    Purpose To describe patterns of purging and binge eating from early through late adolescence in female and male youth across a range of sexual orientations. Methods Using data from the prospective Growing Up Today Study, a large cohort of U.S. youth, we investigated trends in past-year self-reports of purging (ever vomit or use laxatives for weight control) and binge eating at least monthly. The analytic sample included 57,668 observations from repeated measures gathered from 13,795 youth ages 12 to 23 years providing information collected by self-administered questionnaires from six waves of data collection. We used multivariable logistic regression models to examine sexual orientation group (heterosexual, “mostly heterosexual,” bisexual, and lesbian/gay) differences in purging and binge eating throughout adolescence, with same-gender heterosexuals as the referent group and controlling for age and race/ethnicity. Results Throughout adolescence, in most cases, sexual orientation group differences were evident at the youngest ages and persisted through adolescence. Among females and compared to heterosexuals, “mostly heterosexuals,” bisexuals, and lesbians were more likely to report binge eating, but only “mostly heterosexuals” and bisexuals were also more likely to report purging. Among males, all three sexual orientation subgroups were more likely than heterosexual males to report both binge eating and purging. Within each orientation subgroup, females generally reported higher prevalence of purging and binge eating than did males. Conclusions Clinicians need to be alert to the risk of eating disordered behaviors in lesbian, gay, bisexual, and “mostly heterosexual” adolescents of both genders in order to better evaluate these youth and refer them for treatment. PMID:19699419

  9. The Initial Purging Policies after the 1965 Incident at Lubang Buaya

    Directory of Open Access Journals (Sweden)

    Yosef Djakababa

    2013-01-01

    Full Text Available After the Lubang Buaya incident on 1 October 1965 in which six top Indonesian Army generals and a lieutenant were killed, the Army began to implement a nationwide purging campaign with the assistance of civilian anti-communist groups. Thousands of PKI members, supporters and pro-Sukarno groups/individuals immediately became the target of this purge. For organisational purposes, several purging policies were released and then strictly enforced. The official purging policies that are highlighted in this paper are a series of initial directives that were released within days of the generals’ executions. They do not explicitly translate into orders to kill, but are more of a guideline to help anti-communist officials classify and contain communists and other PKI followers. This article attempts to show how these initial directives evolved and also discusses competing purge policies from non-military sources. The co-existence and overlapping nature of the various directives indicate that a power struggle existed between the anti-communist group led by General Soeharto and the presidium of the Dwikora Cabinet who were loyal to President Soekarno.

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

    Science.gov (United States)

    Wright, Bob W; Wright, Cherylyn W

    2012-10-26

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

  11. Evolution in miniaturized column liquid chromatography instrumentation and applications: An overview.

    Science.gov (United States)

    Nazario, Carlos E D; Silva, Meire R; Franco, Maraíssa S; Lanças, Fernando M

    2015-11-20

    The purpose of this article is to underline the miniaturized LC instrumental system and describe the evolution of commercially available systems by discussing their advantages and drawbacks. Nowadays, there are already many miniaturized LC systems available with a great variety of pump design, interface and detectors as well as efficient columns technologies and reduced connections devices. The solvent delivery systems are able to drive the mobile phase without flow splitters and promote gradient elution using either dual piston reciprocating or syringe-type pumps. The mass spectrometry as detection system is the most widely used detection system; among many alternative ionization sources direct-EI LC-MS is a promising alternative to APCI. In addition, capillary columns are now available showing many possibilities of stationary phases, inner diameters and hardware materials. This review provides a discussion about miniaturized LC demonstrating fundamentals and instrumentals' aspects of the commercially available miniaturized LC instrumental system mainly nano and micro LC formats. This review also covers the recent developments and trends in instrumentation, capillary and nano columns, and several applications of this very important and promising field. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Ultra narrow bore thick film capillaries for microcolumn separations. Part 1. GC experiments

    NARCIS (Netherlands)

    Steenackers, D.; Sandra, P.J.F.; Sandra, P.; Devos, G.

    1993-01-01

    Ultra narrow bore (50 mum 1.0.) fused silica columns were statically coated with apolar stationary phases to obtain beta values ranging from 6.25 to 50 (filmthickness 2 to 0.25 mum). Performance of the 1 and 2 mum columns in Capillary Gas Chromatography (CGC) is highlighted.

  13. Air riding seal with purge cavity

    Science.gov (United States)

    Sexton, Thomas D; Mills, Jacob A

    2017-08-15

    An air riding seal for a turbine in a gas turbine engine, where an annular piston is axial moveable within an annular piston chamber formed in a stator of the turbine and forms a seal with a surface on the rotor using pressurized air that forms a cushion in a pocket of the annular piston. A purge cavity is formed on the annular piston and is connected to a purge hole that extends through the annular piston to a lower pressure region around the annular piston or through the rotor to an opposite side. The annular piston is sealed also with inner and outer seals that can be a labyrinth seal to form an additional seal than the cushion of air in the pocket to prevent the face of the air riding seal from overheating.

  14. Exploitation of a microporous organic polymer as a stationary phase for capillary gas chromatography

    International Nuclear Information System (INIS)

    Lu, Cuiming; Liu, Shuqin; Xu, Jianqiao; Ding, Yajuan; Ouyang, Gangfeng

    2016-01-01

    Microporous organic polymers (MOPs) have emerged as a new class of functional porous materials with unique characteristics and potential uses in diverse areas. However, the field of MOPs for gas chromatographic (GC) separations has not been well explored. Herein, a MOP namely KAPs-1 was dynamic coated onto a capillary column for the first time. The fabricated column exhibited a nonpolar nature and the column efficiency for n-dodecane was up to 7769 plates m"−"1. The KAPs-1 coated column showed high GC separation performance for a series of volatile organic compounds (VOCs) including the challenging ethylbenzene and xylene isomers, which could not be resolved at baseline on the commercial 5% phenyl polysiloxane stationary phase. Moreover, the relative standard deviations for five replicate determinations of the studied analytes were 0.0–0.6%, 0.9–3.2%, 1.1–5.9%, 0.8–3.7% for retention time, peak area, peak height and peak width, respectively. To investigate the interaction between some analytes and the stationary phase, thermodynamic and kinetic parameters were also evaluated. The results of this study show it is very promising to utilize MOPs as stationary phases for capillary GC. - Highlights: • A microporous organic polymer was explored as a novel stationary phase for capillary GC. • The column showed high separation performance for VOCs including the challenging ethylbenzene and xylene isomers. • Thermodynamic and kinetic parameters for BTEXs were determined to study the analyte-stationary phase interaction.

  15. Stable carbon and hydrogen isotope analysis of methyl tert-butyl ether and tert-amyl methyl ether by purge and trap-gas chromatography-isotope ratio mass spectrometry: method evaluation and application.

    Science.gov (United States)

    Kujawinski, Dorothea M; Stephan, Manuel; Jochmann, Maik A; Krajenke, Karen; Haas, Joe; Schmidt, Torsten C

    2010-01-01

    In order to monitor the behaviour of contaminants in the aqueous environment effective enrichment techniques often have to be employed due to their low concentrations. In this work a robust and sensitive purge and trap-gas chromatography-isotope ratio mass spectrometry method for carbon and hydrogen isotope analysis of fuel oxygenates in water is presented. The method evaluation included the determination of method detection limits, accuracy and reproducibility of deltaD and delta(13)C values. Lowest concentrations at which reliable delta(13)C values could be determined were 5 microg L(-1) and 28 microg L(-1) for TAME and MTBE, respectively. Stable deltaD values for MTBE and TAME could be achieved for concentrations as low as 25 and 50 microg L(-1). Good long-term reproducibility of delta(13)C and deltaD values was obtained for all target compounds. But deltaD values varying more than 5 per thousand were observed using different thermal conversion tubes. Thus, a correction of deltaD values in the analysis of groundwater samples was necessary to guarantee comparability of the results. The applicability of this method was shown by the analysis of groundwater samples from a gasoline contaminated site. By two dimensional isotope analysis two locations within this site were identified at which anaerobic and aerobic degradation of methyl tert-butyl ether occurred.

  16. Escherichia coli adhesive coating as a chiral stationary phase for open tubular capillary electrochromatography enantioseparation

    Energy Technology Data Exchange (ETDEWEB)

    Fu, Qifeng, E-mail: fuqifeng1990@163.com [Department of Medicinal Chemistry, Southwest Medical University, Luzhou 646000 (China); Zhang, Kailian; Gao, Die; Wang, Lujun [Department of Medicinal Chemistry, Southwest Medical University, Luzhou 646000 (China); Yang, Fengqing; Liu, Yao [School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030 (China); Xia, Zhining, E-mail: tcm_anal_cqu@163.com [Innovative Drug Research Centre and School of Pharmaceutical Sciences, Chongqing University, Chongqing 400030 (China); School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030 (China)

    2017-05-29

    Bacteria, the microorganism with intrinsic chirality, have numerous fascinating chiral phenomena such as various chirality-triggered biological processes and behaviors. Herein, bacteria were firstly explored as novel chiral stationary phases in open-tubular capillary electrochromatography (OT-CEC) for enantioseparation of fluoroquinolone enantiomers and simultaneous separation of six fluoroquinolone antibiotics. The model strain, i.e. non-pathogenic Escherichia coli (E. coli) DH5α, was adhered onto the inner surface of positively charged polyethyleneimine (PEI) modified capillaries based on the bacterial adhesion characteristics and strong electrostatic interaction. The morphology and thickness of the bacteria adhesive coatings in the capillary were characterized by field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). Baseline separation of ofloxacin and partial separation of lomefloxacin enantiomers could be achieved by the E. coli coated columns. The preparation parameters including the coating time and concentration of bacteria that affecting the chiral resolution were intensively investigated. The electrophoretic parameters, including pH, buffer concentration and applied voltage, were also optimized. The developed method was validated (linearity, LOD, LOQ, intra-day, inter-day and column-to-column repeatability and recovery) and successfully utilized for the quantitative analysis of ofloxacin enantiomers in the ofloxacin tablets. Moreover, only a slight decrease in the separation efficiency was observed after 90 consecutive runs on the E. coli@capillary. These results demonstrated that bacteria are promising stationary phases for chiral separation in CEC. - Highlights: • Bacteria were firstly introduced in OT-CEC as a chiral stationary phase for chiral separation. • Enantioseparation of ofloxacin enantiomers was achieved on E. coli coated open tubular capillary column. • Bacterial stationary phases may be used to

  17. Escherichia coli adhesive coating as a chiral stationary phase for open tubular capillary electrochromatography enantioseparation

    International Nuclear Information System (INIS)

    Fu, Qifeng; Zhang, Kailian; Gao, Die; Wang, Lujun; Yang, Fengqing; Liu, Yao; Xia, Zhining

    2017-01-01

    Bacteria, the microorganism with intrinsic chirality, have numerous fascinating chiral phenomena such as various chirality-triggered biological processes and behaviors. Herein, bacteria were firstly explored as novel chiral stationary phases in open-tubular capillary electrochromatography (OT-CEC) for enantioseparation of fluoroquinolone enantiomers and simultaneous separation of six fluoroquinolone antibiotics. The model strain, i.e. non-pathogenic Escherichia coli (E. coli) DH5α, was adhered onto the inner surface of positively charged polyethyleneimine (PEI) modified capillaries based on the bacterial adhesion characteristics and strong electrostatic interaction. The morphology and thickness of the bacteria adhesive coatings in the capillary were characterized by field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). Baseline separation of ofloxacin and partial separation of lomefloxacin enantiomers could be achieved by the E. coli coated columns. The preparation parameters including the coating time and concentration of bacteria that affecting the chiral resolution were intensively investigated. The electrophoretic parameters, including pH, buffer concentration and applied voltage, were also optimized. The developed method was validated (linearity, LOD, LOQ, intra-day, inter-day and column-to-column repeatability and recovery) and successfully utilized for the quantitative analysis of ofloxacin enantiomers in the ofloxacin tablets. Moreover, only a slight decrease in the separation efficiency was observed after 90 consecutive runs on the E. coli@capillary. These results demonstrated that bacteria are promising stationary phases for chiral separation in CEC. - Highlights: • Bacteria were firstly introduced in OT-CEC as a chiral stationary phase for chiral separation. • Enantioseparation of ofloxacin enantiomers was achieved on E. coli coated open tubular capillary column. • Bacterial stationary phases may be used to

  18. Biodegradation of phenol, salicylic acid, benzenesulfonic acid, and iomeprol by Pseudomonas fluorescens in the capillary fringe.

    Science.gov (United States)

    Hack, Norman; Reinwand, Christian; Abbt-Braun, Gudrun; Horn, Harald; Frimmel, Fritz H

    2015-12-01

    Mass transfer and biological transformation phenomena in the capillary fringe were studied using phenol, salicylic acid, benzenesulfonic acid, and the iodinated X-ray contrast agent iomeprol as model organic compounds and the microorganism strain Pseudomonas fluorescens. Three experimental approaches were used: Batch experiments (uniform water saturation and transport by diffusion), in static columns (with a gradient of water saturation and advective transport in the capillaries) and in a flow-through cell (with a gradient of water saturation and transport by horizontal and vertical flow: 2-dimension flow-through microcosm). The reactors employed for the experiments were filled with quartz sand of defined particle size distribution (dp=200...600 μm, porosity ε=0.42). Batch experiments showed that phenol and salicylic acid have a high, whereas benzenesulfonic acid and iomeprol have a quite low potential for biodegradation under aerobic conditions and in a matrix nearly close to water saturation. Batch experiments under anoxic conditions with nitrate as electron acceptor revealed that the biodegradation of the model compounds was lower than under aerobic conditions. Nevertheless, the experiments showed that the moisture content was also responsible for an optimized transport in the liquid phase of a porous medium. Biodegradation in the capillary fringe was found to be influenced by both the moisture content and availability of the dissolved substrate, as seen in static column experiments. The gas-liquid mass transfer of oxygen also played an important role for the biological activity. In static column experiments under aerobic conditions, the highest biodegradation was found in the capillary fringe (e.g. βt/β0 (phenol)=0 after t=6 d) relative to the zone below the water table and unsaturated zone. The highest biodegradation occurred in the flow-through cell experiment where the height of the capillary fringe was largest. Copyright © 2015 Elsevier B.V. All rights

  19. Voltage-assisted capillary LC of peptides using monolithic capillary columns prepared by ring-opening metathesis polymerization

    Czech Academy of Sciences Publication Activity Database

    Sedláková, Pavla; Mikšík, Ivan; Gatschelhofer, Ch.; Sinner, F. M.; Buchmeiser, M. R.

    2007-01-01

    Roč. 28, č. 13 (2007), s. 2219-2222 ISSN 0173-0835 R&D Projects: GA ČR GA203/05/2539; GA ČR GA203/06/1044; GA MŠk(CZ) 1M0510 Institutional research plan: CEZ:AV0Z50110509 Keywords : ROMP * voltage-assisted capillary LC Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.609, year: 2007

  20. Purged window apparatus. [On-line spectroscopic analysis of gas flow systems

    Science.gov (United States)

    Ballard, E.O.

    1982-04-05

    A purged window apparatus is described which utilizes tangentially injected heated purge gases in the vicinity of electromagnetic radiation transmitting windows and a tapered external mounting tube to accelerate these gases to provide a vortex flow on the window surface and a turbulent flow throughout the mounting tube thereby preventing backstreaming of flowing gases under investigation in a chamber to which a plurality of similar purged apparatus is attached with the consequent result that spectroscopic analyses can be undertaken for lengthy periods without the necessity of interrupting the flow for cleaning or replacing the windows due to contamination.

  1. On-line Automated Sample Preparation-Capillary Gas Chromatography for the Analysis of Plasma Samples.

    NARCIS (Netherlands)

    Louter, A.J.H.; van der Wagt, R.A.C.A.; Brinkman, U.A.T.

    1995-01-01

    An automated sample preparation module, (the automated sample preparation with extraction columns, ASPEC), was interfaced with a capillary gas chromatograph (GC) by means of an on-column interface. The system was optimised for the determination of the antidepressant trazodone in plasma. The clean-up

  2. Aquifer restoration system improvement using an acid fluid purge

    International Nuclear Information System (INIS)

    Hodder, E.A.; Peck, C.A.

    1992-01-01

    The implementation of a water pump acid purge procedure at a free-phase liquid hydrocarbon recovery site has increased water pump operational run times and improved the effectiveness of the aquifer restoration effort. Before introduction of this technique, pumps at some locations would fail within 14 days of operation due to CaSO 4 .2H 2 O (calcium sulfate) precipitate fouling. After acid purge implementation at these locations, pump operational life improved to an average of over 110 days. Other locations, where pump failures would occur within one month, were improved to approximately six months of operation. The increase in water pump run time has also improved the liquid hydrocarbon recovery rate by 2,000 gallons per day; representing a 20% increase for the aquifer restoration system. Other concepts tested in attempts to prolong pump life included: specially designed electric submersible pumps, submersible pump shrouds intended to reduce the fluid pressure shear that enhances CaSO 4 .2H 2 O precipitation, and high volume pneumatic gas lift pumps. Due to marginal pump life improvement or other undesirable operational features, these concepts were primarily ineffective. The purge apparatus utilizes an acid pump, hose, and discharge piping to deliver the solution directly into the inlet of an operating water pump. The water pumps used for this activity require stainless steel construction with Teflon or other acid resistant bearings and seals. Purges are typically conducted before sudden discharge pressure drops (greater than 15 psig) occur for the operating water pump. Depending on volume of precipitate accumulation and pump type, discharge pressure is restored after introduction of 10 to 40 gallons of hydrochloric acid solution. The acid purge procedure outlined herein eliminates operational downtime and does not require well head pump removal and the associated costs of industry cleaning procedures

  3. Meniscus formation in a capillary and the role of contact line friction.

    Science.gov (United States)

    Andrukh, Taras; Monaenkova, Daria; Rubin, Binyamin; Lee, Wah-Keat; Kornev, Konstantin G

    2014-01-28

    We studied spontaneous formation of an internal meniscus by dipping glass capillaries of 25 μm to 350 μm radii into low volatile hexadecane and tributyl phosphate. X-ray phase contrast and high speed optical microscopy imaging were employed. We showed that the meniscus completes its formation when the liquid column is still shorter than the capillary radius. After that, the meniscus travels about ten capillary radii at a constant velocity. We demonstrated that the experimental observations can be explained by introducing a friction force linearly proportional to the meniscus velocity with a friction coefficient depending on the air/liquid/solid triplet. It was demonstrated that the friction coefficient does not depend on the capillary radius. Numerical solution of the force balance equation revealed four different uptake regimes that can be specified in a phase portrait. This phase portrait was found to be in good agreement with the experimental results and can be used as a guide for the design of thin porous absorbers.

  4. Evaluation of CP sil 8 film thickness for the capillary GC analysis of methyl mercury

    DEFF Research Database (Denmark)

    Petersen, Jens Højslev; Drabæk, Iver

    1992-01-01

    Different commercially available CP-Sil 8 CB capillary columns have been tested with a mixed standard containing methyl mercury chloride, ethyl mercury chloride and a stable nonpolar chlorinated hydrocarbon. The aim of the study was to see whether the columns tested could be used without special...... available insert for on-column injections on wide bore columns, and a 5.35 mum thick stationary phase. It was concluded that this CP Sil 8 CB column gave good results although minor interactions between the organo-mercury compounds and the column could be seen....

  5. Interior Temperature Measurement Using Curved Mercury Capillary Sensor Based on X-ray Radiography

    Science.gov (United States)

    Chen, Shuyue; Jiang, Xing; Lu, Guirong

    2017-07-01

    A method was presented for measuring the interior temperature of objects using a curved mercury capillary sensor based on X-ray radiography. The sensor is composed of a mercury bubble, a capillary and a fixed support. X-ray digital radiography was employed to capture image of the mercury column in the capillary, and a temperature control system was designed for the sensor calibration. We adopted livewire algorithms and mathematical morphology to calculate the mercury length. A measurement model relating mercury length to temperature was established, and the measurement uncertainty associated with the mercury column length and the linear model fitted by least-square method were analyzed. To verify the system, the interior temperature measurement of an autoclave, which is totally closed, was taken from 29.53°C to 67.34°C. The experiment results show that the response of the system is approximately linear with an uncertainty of maximum 0.79°C. This technique provides a new approach to measure interior temperature of objects.

  6. Analysis of multiple quaternary ammonium compounds in the brain using tandem capillary column separation and high resolution mass spectrometric detection.

    Science.gov (United States)

    Falasca, Sara; Petruzziello, Filomena; Kretz, Robert; Rainer, Gregor; Zhang, Xiaozhe

    2012-06-08

    Endogenous quaternary ammonium compounds are involved in various physiological processes in the central nervous system. In the present study, eleven quaternary ammonium compounds, including acetylcholine, choline, carnitine, acetylcarnitine and seven other acylcarnitines of low polarity, were analyzed from brain extracts using a two dimension capillary liquid chromatography-Fourier transform mass spectrometry method. To deal with their large difference in hydrophobicities, tandem coupling between reversed phase and hydrophilic interaction chromatography columns was used to separate all the targeted quaternary ammonium compounds. Using high accuracy mass spectrometry in selected ion monitoring mode, all the compounds could be detected from each brain sample with high selectivity. The developed method was applied for the relative quantification of these quaternary ammonium compounds in three different brain regions of tree shrews: prefrontal cortex, striatum, and hippocampus. The comparative analysis showed that quaternary ammonium compounds were differentially distributed across the three brain areas. The analytical method proved to be highly sensitive and reliable for simultaneous determination of all the targeted analytes from brain samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. Preparation of hydrophilic monolithic capillary column by in situ photo-polymerization of N-vinyl-2-pyrrolidinone and acrylamide for highly selective and sensitive enrichment of N-linked glycopeptides.

    Science.gov (United States)

    Jiang, Hao; Yuan, Huiming; Qu, Yanyan; Liang, Yu; Jiang, Bo; Wu, Qi; Deng, Nan; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

    2016-01-01

    In this study, a novel kind of amide functionalized hydrophilic monolith was synthesized by the in situ photo-polymerization of N-vinyl-2-pyrrolidinone (NVP), acrylamide (AM), and N, N'-methylenebisacrylamide (MBA) in a UV transparent capillary, and successfully applied for hydrophilic interaction chromatography (HILIC) based enrichment of N-linked glycopeptides. With 2 μg of the tryptic digests of IgG as the sample, after enrichment, 18 glycopeptides could be identified by MALDI-TOF/TOF MS analysis. Furthermore, with the mixture of BSA and IgG digests (10,000:1, m/m) as the sample, 6 N-linked glycopeptides were unambiguously identified after enrichment, indicating the high selectivity and good specificity of such material. Moreover, such a monolithic capillary column was also applied for the N-glycosylation sites profiling of 6 μg protein digests from HeLa cells and 1 μL human serum. In total, 530 and 262 unique N-glycosylated peptides were identified, respectively, corresponding to 282 and 124N-glycoproteins, demonstrating its great potential for the large scale glycoproteomics analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Exploitation of a microporous organic polymer as a stationary phase for capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Cuiming; Liu, Shuqin; Xu, Jianqiao; Ding, Yajuan; Ouyang, Gangfeng, E-mail: cesoygf@mail.sysu.edu.cn

    2016-01-01

    Microporous organic polymers (MOPs) have emerged as a new class of functional porous materials with unique characteristics and potential uses in diverse areas. However, the field of MOPs for gas chromatographic (GC) separations has not been well explored. Herein, a MOP namely KAPs-1 was dynamic coated onto a capillary column for the first time. The fabricated column exhibited a nonpolar nature and the column efficiency for n-dodecane was up to 7769 plates m{sup −1}. The KAPs-1 coated column showed high GC separation performance for a series of volatile organic compounds (VOCs) including the challenging ethylbenzene and xylene isomers, which could not be resolved at baseline on the commercial 5% phenyl polysiloxane stationary phase. Moreover, the relative standard deviations for five replicate determinations of the studied analytes were 0.0–0.6%, 0.9–3.2%, 1.1–5.9%, 0.8–3.7% for retention time, peak area, peak height and peak width, respectively. To investigate the interaction between some analytes and the stationary phase, thermodynamic and kinetic parameters were also evaluated. The results of this study show it is very promising to utilize MOPs as stationary phases for capillary GC. - Highlights: • A microporous organic polymer was explored as a novel stationary phase for capillary GC. • The column showed high separation performance for VOCs including the challenging ethylbenzene and xylene isomers. • Thermodynamic and kinetic parameters for BTEXs were determined to study the analyte-stationary phase interaction.

  9. An all-glass solid sampling device for open tubular columns in gas chromatography

    NARCIS (Netherlands)

    Cox, T.P.H.; vd Berg, P.M.J.

    1972-01-01

    An all-glass system for direct sample-introduction of high-boiling compounds onto open tubular columns is described. The standard deviation for quantitative measurements is less than 2.7%. The loss in resolving power of capillary columns, due to this injection system is negligible. The system is

  10. Dynamic stability of a lightly damped column trapped by a ...

    African Journals Online (AJOL)

    In this paper we initiate an analytical approach for determining the dynamic buckling load of a finite viscously damped column acted upon by a harmonically slowly varying explicitly time dependent load. The viscous damping is considered light and the column rests on an elastic foundation that produces a nonlinear ...

  11. Evaluation of the Purge Water Management System (PWMS) monitor well sampling technology at SRS

    International Nuclear Information System (INIS)

    Hiergesell, R.A.; Cardoso-Neto, J.E.; Williams, D.W.

    1997-01-01

    Due to the complex issues surrounding Investigation Derived Waste (IDW) at SRS, the Environmental Restoration Division has been exploring new technologies to deal with the purge water generated during monitoring well sampling. Standard procedures for sampling generates copious amounts of purge water that must be managed as hazardous waste, when containing hazardous and/or radiological contaminants exceeding certain threshold levels. SRS has obtained Regulator approval to field test an innovative surface release prevention mechanism to manage purge water. This mechanism is referred to as the Purge Water Management System (PWMS) and consists of a collapsible bladder situated within a rigid metal tank

  12. Tunable thick porous silica coating fabricated by multilayer-by-multilayer bonding of silica nanoparticles for open-tubular capillary chromatographic separation.

    Science.gov (United States)

    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.

  13. Incorporating the Impacts of Small Scale Rock Heterogeneity into Models of Flow and Trapping in Target UK CO2 Storage Systems

    Science.gov (United States)

    Jackson, S. J.; Reynolds, C.; Krevor, S. C.

    2017-12-01

    Predictions of the flow behaviour and storage capacity of CO2 in subsurface reservoirs are dependent on accurate modelling of multiphase flow and trapping. A number of studies have shown that small scale rock heterogeneities have a significant impact on CO2flow propagating to larger scales. The need to simulate flow in heterogeneous reservoir systems has led to the development of numerical upscaling techniques which are widely used in industry. Less well understood, however, is the best approach for incorporating laboratory characterisations of small scale heterogeneities into models. At small scales, heterogeneity in the capillary pressure characteristic function becomes significant. We present a digital rock workflow that combines core flood experiments with numerical simulations to characterise sub-core scale capillary pressure heterogeneities within rock cores from several target UK storage reservoirs - the Bunter, Captain and Ormskirk sandstone formations. Measured intrinsic properties (permeability, capillary pressure, relative permeability) and 3D saturations maps from steady-state core flood experiments were the primary inputs to construct a 3D digital rock model in CMG IMEX. We used vertical end-point scaling to iteratively update the voxel by voxel capillary pressure curves from the average MICP curve; with each iteration more closely predicting the experimental saturations and pressure drops. Once characterised, the digital rock cores were used to predict equivalent flow functions, such as relative permeability and residual trapping, across the range of flow conditions estimated to prevail in the CO2 storage reservoirs. In the case of the Captain sandstone, rock cores were characterised across an entire 100m vertical transect of the reservoir. This allowed analysis of the upscaled impact of small scale heterogeneity on flow and trapping. Figure 1 shows the varying degree to which heterogeneity impacted flow depending on the capillary number in the

  14. Measurements of the purge helium pressure drop across pebble beds packed with lithium orthosilicate and glass pebbles

    Energy Technology Data Exchange (ETDEWEB)

    Abou-Sena, Ali, E-mail: ali.abou-sena@kit.edu; Arbeiter, Frederik; Boccaccini, Lorenzo V.; Schlindwein, Georg

    2014-10-15

    Highlights: • The objective is to measure the purge helium pressure drop across various HCPB-relevant pebble beds packed with lithium orthosilicate and glass pebbles. • The purge helium pressure drop significantly increases with decreasing the pebbles diameter from one run to another. • At the same superficial velocity, the pressure drop is directly proportional to the helium inlet pressure. • The Ergun's equation can successfully model the purge helium pressure drop for the HCPB-relevant pebble beds. • The measured values of the purge helium pressure drop for the lithium orthosilicate pebble bed will support the design of the purge gas system for the HCPB breeder units. - Abstract: The lithium orthosilicate pebble beds of the Helium Cooled Pebble Bed (HCPB) blanket are purged by helium to transport the produced tritium to the tritium extraction system. The pressure drop of the purge helium has a direct impact on the required pumping power and is a limiting factor for the purge mass flow. Therefore, the objective of this study is to measure the helium pressure drop across various HCPB-relevant pebble beds packed with lithium orthosilicate and glass pebbles. The pebble bed was formed by packing the pebbles into a stainless steel cylinder (ID = 30 mm and L = 120 mm); then it was integrated into a gas loop that has four variable-speed side-channel compressors to regulate the helium mass flow. The static pressure was measured at two locations (100 mm apart) along the pebble bed and at inlet and outlet of the pebble bed. The results demonstrated that: (i) the pressure drop significantly increases with decreasing the pebbles diameter, (ii) for the same superficial velocity, the pressure drop is directly proportional to the inlet pressure, and (iii) predictions of Ergun's equation agree well with the experimental results. The measured pressure drop for the lithium orthosilicate pebble bed will support the design of the purge gas system for the HCPB.

  15. Center column design of the PLT

    International Nuclear Information System (INIS)

    Citrolo, J.; Frankenberg, J.

    1975-01-01

    The center column of the PLT machine is a secondary support member for the toroidal field coils. Its purpose is to decrease the bending moment at the nose of the coils. The center column design was to have been a stainless steel casting with the toroidal field coils grouped around the casting at installation, trapping it in place. However, the castings developed cracks during fabrication and were unsuitable for use. Installation of the coils proceeded without the center column. It then became necessary to redesign a center column which would be capable of installation with the toroidal field coils in place. The final design consists of three A-286 forgings. This paper discusses the final center column design and the influence that new knowledge, obtained during the power tests, had on the new design

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

    Science.gov (United States)

    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.

  17. Application of a diode-array detector in capillary electrophoresis

    NARCIS (Netherlands)

    Beck, W.; Hoek, van R.; Engelhardt, H.

    1993-01-01

    In the last decade diode-array detection has proved to be extremely useful in high performance liquid chromatography in recording UV-visible spectra directly and on-line in the column effluent. In capillary electrophoresis (CE) only fast-scanning detectors with long scan times (up to 2 s) are

  18. New separation and detection methods in capillary electrophoresis and ion chromatography for the analysis of ionic compounds

    International Nuclear Information System (INIS)

    Mayrhofer, K.

    1999-10-01

    The first part of the thesis deals with the simultaneous analysis of inorganic anions and organic acids in electrodeposition coatings with the co-electroosmotic capillary electrophoresis. The coating of workpieces, e.g. car bodies, by means of an electrodeposition process is an important methodology especially in the automotiv industries. It is usually performed by introducing the object into a basin filled with a water-based electro-dipcoat, applying a voltage of 200-400 Volts (direct current) and using the bodywork as cathode. Because the workpiece has to pass a number of preliminary treatments before the coating procedure, ionic compound may be carried into the basin. If the concentrations of these ionic impurities is too high, the electro-deposition of the binding agent fails or the thickness of the coating is not reproducible. The organic acids are used as neutralization agents in order to control and to keep the pH of the basin constant. The common method of analysing ionic impurities is ion chromatography. The organic acids have to be separated in an ion exclusion chromatography column because organic acids may coelute with the inorganic anions or elute with the dead volume. Therefore a separation method for capillary electrophoresis was developed which enables the simultaneouse analysis of inorganic anions and organic acids in less then 5 minutes. Chloride, nitrate, sulfate, fuoride, phosphate, carbonate, formic acid, acetic acid, lactic acid and butyric acid were detected with indirect UV-detection at 254 nm. For removal of the the binding agent and the pigments the lacquer was mixed with a 0.01 M sodium hydroxide solution and then filtered through a 0.45 μm filter cartridge. 5 mM trimellitic acid, titrated with sodium hydroxid to pH 10, 0.001 % hexadimethrinbromide and 20 % acetonitrile served as buffer. The analytes were separated with a satisfactory resolution. Between every analysis the fused silica capillary was purged for two minutes with buffer. So

  19. Design and Operation of Cryogenic Distillation Research Column for Ultra-Low Background Experiments

    Science.gov (United States)

    Chiller, Christopher; Alanson Chiller, Angela; Jasinski, Benjamin; Snyder, Nathan; Mei, Dongming

    2013-04-01

    Motivated by isotopically enriched germanium (76Ge and 73Ge) for monocrystalline crystal growth for neutrinoless double-beta decay and dark matter experiments, a cryogenic distillation research column was developed. Without market availability of distillation columns in the temperature range of interest with capabilities necessary for our purposes, we designed, fabricated, tested, refined and operated a two-meter research column for purifying and separating gases in the temperature range from 100-200K. Due to interest in defining stratification, purity and throughput optimization, capillary lines were integrated at four equidistant points along the length of the column such that real-time residual gas analysis could guide the investigation. Interior gas column temperatures were monitored and controlled within 0.1oK accuracy at the top and bottom. Pressures were monitored at the top of the column to four significant figures. Subsequent impurities were measured at partial pressures below 2E-8torr. We report the performance of the column in this paper.

  20. Comparison of dialysis membrane diffusion samplers and two purging methods in bedrock wells

    Science.gov (United States)

    Imbrigiotta, T.E.; Ehlke, T.A.; Lacombe, P.J.; Dale, J.M.; ,

    2002-01-01

    Collection of ground-water samples from bedrock wells using low-flow purging techniques is problematic because of the random spacing, variable hydraulic conductivity, and variable contamination of contributing fractures in each well's open interval. To test alternatives to this purging method, a field comparison of three ground-water-sampling techniques was conducted on wells in fractured bedrock at a site contaminated primarily with volatile organic compounds. Constituent concentrations in samples collected with a diffusion sampler constructed from dialysis membrane material were compared to those in samples collected from the same wells with a standard low-flow purging technique and a hybrid (high-flow/low-flow) purging technique. Concentrations of trichloroethene, cis-1,2-dichloroethene, vinyl chloride, calcium, chloride, and alkalinity agreed well among samples collected with all three techniques in 9 of the 10 wells tested. Iron concentrations varied more than those of the other parameters, but their pattern of variation was not consistent. Overall, the results of nonparametric analysis of variance testing on the nine wells sampled twice showed no statistically significant difference at the 95-percent confidence level among the concentrations of volatile organic compounds or inorganic constituents recovered by use of any of the three sampling techniques.

  1. Human reliability analysis for In-Tank Precipitation alignment and startup of emergency purge ventilation equipment

    International Nuclear Information System (INIS)

    Olsen, L.M.

    1993-08-01

    This report documents the methodology used for calculating the human error probability for establishing air based ventilation using emergency purge ventilation equipment on In-Tank Precipitation (ITP) processing tanks 48 and 49 after a failure of the nitrogen purge system following a seismic event. The analyses were performed according to THERP (Technique for Human Error Rate Prediction). The calculated human error probabilities are provided as input to the Fault Tree Analysis for the ITP Nitrogen Purge System. The analysis assumes a seismic event initiator leading to establishing air based ventilation on the ITP processing tanks 48 and 49. At the time of this analysis only the tanks and the emergency purge ventilation equipment are seismically qualified. Consequently, onsite and offsite power is assumed to be unavailable and all operator control actions are to be performed locally on the tank top. Assumptions regarding procedures, staffing, equipment locations, equipment tagging, equipment availability, and training were made and are documented in this report. The human error probability for establishing air based ventilation using the emergency purge ventilation equipment on In-Tank Precipitation processing tanks 48 and 49 after a failure of the nitrogen purge system following a seismic event is 4.2E-6 (median value on the lognormal scale). It is important to note that this result is predicated on the implementation of all of the assumptions listed in the ''Assumptions'' section of this report. This analysis was not based on the current conditions in ITP. The analysis is to be used as a tool to aid ITP operations personnel in achieving the training, procedural, and operational goals outlined in this document

  2. Purge Procedures and Leak Testing for the Morgan Breathing System (MBS) 2000 Closed-Circuit Oxygen Rebreather

    National Research Council Canada - National Science Library

    Fothergill, David

    2005-01-01

    .... Since purging accounts for most of the O2 used when breathing on the MBS 2000, optimizing the purge procedure will maximize the duration of the O2 supply and minimize oxygen leaks into the chamber atmosphere...

  3. Gas dispersion concentration of trace inorganic contaminants from fuel gas and analysis using head-column field-amplified sample stacking capillary electrophoresis.

    Science.gov (United States)

    Yang, Jianmin; Li, Hai-Fang; Li, Meilan; Lin, Jin-Ming

    2012-08-21

    The presence of inorganic elements in fuel gas generally accelerates the corrosion and depletion of materials used in the fuel gas industry, and even leads to serious accidents. For identification of existing trace inorganic contaminants in fuel gas in a portable way, a highly efficient gas-liquid sampling collection system based on gas dispersion concentration is introduced in this work. Using the constructed dual path gas-liquid collection setup, inorganic cations and anions were simultaneously collected from real liquefied petroleum gas (LPG) and analyzed by capillary electrophoresis (CE) with indirect UV absorbance detection. The head-column field-amplified sample stacking technique was applied to improve the detection limits to 2-25 ng mL(-1). The developed collection and analytical methods have successfully determined existing inorganic contaminants in a real LPG sample in the range of 4.59-138.69 μg m(-3). The recoveries of cations and anions with spiked LPG samples were between 83.98 and 105.63%, and the relative standard deviations (RSDs) were less than 7.19%.

  4. DEM-CFD simulation of purge gas flow in a solid breeder pebble bed

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Hao [School of Nuclear Science and Technology, University of Science and Technology of China, Hefei 230027 (China); Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); Li, Zhenghong [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); University of Science and Technology of China, Hefei 230027 (China); Guo, Haibing [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); Ye, Minyou [School of Nuclear Science and Technology, University of Science and Technology of China, Hefei 230027 (China); Huang, Hongwen, E-mail: inpclane@sina.com [Institute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China)

    2016-12-15

    Solid tritium breeding blanket applying pebble bed concept is promising for fusion reactors. Tritium bred in the pebble bed is purged out by inert gas. The flow characteristics of the purge gas are important for the tritium transport from the solid breeder materials. In this study, a randomly packed pebble bed was generated by Discrete Element Method (DEM) and verified by radial porosity distribution. The flow parameters of the purge gas in channels were solved by Computational Fluid Dynamics (CFD) method. The results show that the normalized velocity magnitudes have the same damped oscillating patterns with radial porosity distribution. Besides, the bypass flow near the wall cannot be ignored in this model, and it has a slight increase with inlet velocity. Furthermore, higher purging efficiency becomes with higher inlet velocity and especially higher in near wall region.

  5. Development of novel separation techniques for biological samples in capillary electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Huan -Tsung [Iowa State Univ., Ames, IA (United States)

    1994-07-27

    This dissertation includes three different topics: general introduction of capillary electrophoresis (CE); gradient in CE and CE in biological separations; and capillary gel electrophoresis (CGE) for DNA separation. Factors such as temperature, viscosity, pH, and the surface of capillary walls affecting the separation performance are demonstrated. A pH gradient between 3.0 and 5.2 is useful to improve the resolution among eight different organic acids. A flow gradient due to the change in the concentration of surfactant, which is able to coat to the capillary wall to change the flow rate and its direction, is also shown as a good way to improve the resolution for organic compounds. A temperature gradient caused by joule heat is shown by voltage programming to enhance the resolution and shorten the separation time for several phenolic compounds. The author also shows that self-regulating dynamic control of electroosmotic flow in CE by simply running separation in different concentrations of surfactant has less matrix effect on the separation performance. One of the most important demonstrations in this dissertation is that the author proposes on-column reaction which gives several advantages including the use of a small amount of sample, low risk of contamination, and time saving and kinetic features. The author uses this idea with laser induced fluorescence (LIF) as a detection mode to detect an on-column digestion of sub-ng of protein. This technique also is applied to single cell analysis in the group.

  6. AP600 containment purge radiological analysis

    Energy Technology Data Exchange (ETDEWEB)

    O`Connor, M.; Schulz, J.; Tan, C. [Bechtel Power Corporation (United States)] [and others

    1995-02-01

    The AP600 Project is a passive pressurized water reactor power plant which is part of the Design Certification and First-of-a-Kind Engineering effort under the Advanced Light Water Reactor program. Included in this process is the design of the containment air filtration system which will be the subject of this paper. We will compare the practice used by previous plants with the AP600 approach to meet the goals of industry standards in sizing the containment air filtration system. The radiological aspects of design are of primary significance and will be the focus of this paper. The AP600 Project optimized the design to combine the functions of the high volumetric flow rate, low volumetric flow rate, and containment cleanup and other filtration systems into one multi-functional system. This achieves a more simplified, standardized, and lower cost design. Studies were performed to determine the possible concentrations of radioactive material in the containment atmosphere and the effectiveness of the purge system to keep concentrations within 10CFR20 limits and within offsite dose objectives. The concentrations were determined for various reactor coolant system leakage rates and containment purge modes of operation. The resultant concentrations were used to determine the containment accessibility during various stages of normal plant operation including refueling. The results of the parametric studies indicate that a dual train purge system with a capacity of 4,000 cfm per train is more than adequate to control the airborne radioactivity levels inside containment during normal plant operation and refueling, and satisfies the goals of ANSI/ANS-56.6-1986 and limits the amount of radioactive material released to the environment per ANSI/ANS 59.2-1985 to provide a safe environment for plant personnel and offsite residents.

  7. Ultrafast preparation of a polyhedral oligomeric silsesquioxane-based ionic liquid hybrid monolith via photoinitiated polymerization, and its application to capillary electrochromatography of aromatic compounds.

    Science.gov (United States)

    Zhang, Bingyu; Lei, Xiaoyun; Deng, Lijun; Li, Minsheng; Yao, Sicong; Wu, Xiaoping

    2018-06-06

    An ionic liquid hybrid monolithic capillary column was prepared within 7 min via photoinitiated free-radical polymerization of an ionic liquid monomer (1-butyl-3-vinylimidazolium-bis[(trifluoromethyl)sulfonyl]imide); VBIMNTF 2 ) and a methacryl substituted polyhedral oligomeric silsesquioxane (POSS-MA) acting as a cross-linker. The effects of composition of prepolymerization solution and initiation time on the porous structure and electroosmotic flow (EOF) of monolithic column were investigated. The hybrid monolith was characterized by scanning electron microscopy and FTIR. Owing to the introduction of a rigid nanosized POSS silica core and ionic liquids with multiple interaction sites, the monolithic column has a well-defined 3D skeleton morphology, good mechanical stability, and a stable anodic electroosmotic flow. The hybrid monolithic stationary phase was applied to the capillary electrochromatographic separation of various alkylbenzenes, phenols, anilines and polycyclic aromatic hydrocarbons (PAHs). The column efficiency is highest (98,000 plates/m) in case of alkylbenzenes. Mixed-mode retention mechanisms including hydrophobic interactions, π-π stacking, electrostatic interaction and electrophoretic mobility can be observed. This indicates the potential of this material in terms of efficient separation of analytes of different structural type. Graphical Abstract Preparation of a mixed-mode ionic liquid hybrid monolithic column via photoinitiated polymerization of methacryl substituted polyhedral oligomeric silsesquioxane (POSS-MA) and 1-butyl-3-vinylimidazolium-bis[(trifluoromethyl)sulfonyl]imide (VBIMNTF 2 ) ionic liquid for use in capillary electrochromatography.

  8. Improving accuracy and precision of ice core δD(CH4 analyses using methane pre-pyrolysis and hydrogen post-pyrolysis trapping and subsequent chromatographic separation

    Directory of Open Access Journals (Sweden)

    M. Bock

    2014-07-01

    Full Text Available Firn and polar ice cores offer the only direct palaeoatmospheric archive. Analyses of past greenhouse gas concentrations and their isotopic compositions in air bubbles in the ice can help to constrain changes in global biogeochemical cycles in the past. For the analysis of the hydrogen isotopic composition of methane (δD(CH4 or δ2H(CH4 0.5 to 1.5 kg of ice was hitherto used. Here we present a method to improve precision and reduce the sample amount for δD(CH4 measurements in (ice core air. Pre-concentrated methane is focused in front of a high temperature oven (pre-pyrolysis trapping, and molecular hydrogen formed by pyrolysis is trapped afterwards (post-pyrolysis trapping, both on a carbon-PLOT capillary at −196 °C. Argon, oxygen, nitrogen, carbon monoxide, unpyrolysed methane and krypton are trapped together with H2 and must be separated using a second short, cooled chromatographic column to ensure accurate results. Pre- and post-pyrolysis trapping largely removes the isotopic fractionation induced during chromatographic separation and results in a narrow peak in the mass spectrometer. Air standards can be measured with a precision better than 1‰. For polar ice samples from glacial periods, we estimate a precision of 2.3‰ for 350 g of ice (or roughly 30 mL – at standard temperature and pressure (STP – of air with 350 ppb of methane. This corresponds to recent tropospheric air samples (about 1900 ppb CH4 of about 6 mL (STP or about 500 pmol of pure CH4.

  9. Determination of (4-methylcyclohexyl)methanol isomers by heated purge-and-trap GC/MS in water samples from the 2014 Elk River, West Virginia, chemical spill

    Science.gov (United States)

    Foreman, William T.; Rose, Donna L.; Chambers, Douglas B.; Crain, Angela S.; Murtagh, Lucinda K.; Thakellapalli, Haresh; Wang, Kung K.

    2015-01-01

    A heated purge-and-trap gas chromatography/mass spectrometry method was used to determine the cis- and trans-isomers of (4-methylcyclohexyl)methanol (4-MCHM), the reported major component of the Crude MCHM/Dowanol™ PPh glycol ether material spilled into the Elk River upriver from Charleston, West Virginia, on January 9, 2014. The trans-isomer eluted first and method detection limits were 0.16-μg L−1trans-, 0.28-μg L−1cis-, and 0.4-μg L−1 Total (total response of isomers) 4-MCHM. Estimated concentrations in the spill source material were 491-g L−1trans- and 277-g L−1cis-4-MCHM, the sum constituting 84% of the source material assuming its density equaled 4-MCHM. Elk River samples collected ⩽ 3.2 km downriver from the spill on January 15 had low (⩽2.9 μg L−1 Total) 4-MCHM concentrations, whereas the isomers were not detected in samples collected 2 d earlier at the same sites. Similar 4-MCHM concentrations (range 4.2–5.5 μg L−1 Total) occurred for samples of the Ohio River at Louisville, Kentucky, on January 17, ∼630 km downriver from the spill. Total 4-MCHM concentrations in Charleston, WV, office tap water decreased from 129 μg L−1 on January 27 to 2.2 μg L−1on February 3, but remained detectable in tap samples through final collection on February 25 indicating some persistence of 4-MCHM within the water distribution system. One isomer of methyl 4-methylcyclohexanecarboxylate was detected in all Ohio River and tap water samples, and both isomers were detected in the source material spilled.

  10. Capillary electrophoresis in an extended nanospray tip-electrospray as an electrophoretic column

    Czech Academy of Sciences Publication Activity Database

    Týčová, Anna; Foret, František

    2015-01-01

    Roč. 1388, APR (2015), s. 274-279 ISSN 0021-9673 R&D Projects: GA ČR(CZ) GBP206/12/G014 Institutional support: RVO:68081715 Keywords : mass spectrometry * interface * separation * capillary electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2015

  11. Radiological Design Summary Report for TRU Vent and Purge Process

    International Nuclear Information System (INIS)

    Taus, L.B.

    2004-01-01

    This report contains top-level requirements for the various areas of radiological protection for workers. Detailed quotations of the requirements for applicable regulatory documents can be found in the accompanying Implementation Guide. For the purposes of demonstrating compliance with these requirements, per Engineering Standard 01064, shall consider / shall evaluate indicates that the designer must examine the requirement for the design and either incorporate or provide a technical justification as to why the requirement is not incorporated. The Transuranic Vent and Purge process is not a project, but is considered a process change. This process has been performed successfully by Solid Waste on lower activity TRU drums. This summary report applies a graded approach and describes how the Transuranic Vent and Purge process meets each of the applicable radiological design criteria and requirements specified in Manual WSRC-TM-95-1, Engineering Standard Number 01064

  12. Stability and interactions of nanocolloids at fluid interfaces: effects of capillary waves and line tensions

    International Nuclear Information System (INIS)

    Lehle, H; Oettel, M

    2008-01-01

    We analyze the effective potential for nanoparticles trapped at a fluid interface within a simple model which incorporates surface and line tensions as well as a thermal average over interface fluctuations (capillary waves). For a single colloid, a reduced steepness of the potential well hindering movements out of the interface plane compared to rigid interface models is observed, and an instability of the capillary wave partition sum in the case of negative line tensions is pointed out. For two colloids, averaging over the capillary waves leads to an effective Casimir-type interaction which is long ranged, power-like in the inverse distance, but whose power sensitively depends on possible restrictions of the colloid degrees of freedom. A nonzero line tension leads to changes in the magnitude but not in the functional form of the effective potential asymptotics

  13. Long-range particle manipulation in a micro-capillary tube by using a flexural acoustic wave

    International Nuclear Information System (INIS)

    Kim, Eun-Sun; Kim, Nari; Kim, Young-Ho; Lee, Kwang-Jo; Hwang, In-Kag

    2010-01-01

    We report a one-dimensional manipulation of dry Ag particles in micro-capillary tube by using a flexural acoustic wave propagating along the tube. The capillary tube is used as a mechanical guide for both the particles and the acoustic wave, resulting in an effective interaction between them over a long range of 14 cm in length. Linear transport and local trapping of the particles are demonstrated by the excitation of traveling and standing acoustic waves, respectively. The mechanisms for the particle movements are qualitatively explained by frictional forces between the particles and the inner wall of the capillary tube.

  14. Characteristic regional cerebral blood flow patterns in anorexia nervosa patients with binge/purge behavior.

    Science.gov (United States)

    Naruo, T; Nakabeppu, Y; Sagiyama, K; Munemoto, T; Homan, N; Deguchi, D; Nakajo, M; Nozoe, S

    2000-09-01

    The authors' goal was to investigate the effect of imagining food on the regional cerebral blood flow (rCBF) of anorexia nervosa patients with and without habitual binge/purge behavior. The subjects included seven female patients with purely restrictive anorexia, seven female patients with anorexia and habitual binge/purge behavior, and seven healthy women. Single photon emission computed tomography examination was performed before and after the subjects were asked to imagine food. Changes in rCBF count ratios (percent change) were then calculated and compared. The subjects were also asked to assess their degree of fear regarding their control of food intake. The anorexia nervosa patients with habitual binge/purge behavior had a significantly higher percent change in the inferior, superior, prefrontal, and parietal regions of the right brain than the patients with purely restrictive anorexia and the healthy volunteers. The patients with habitual binge/purge behavior also had the highest level of apprehension in regard to food intake. Specific activation in cortical regions suggests an association between habitual binge/purge behavior and the food recognition process linked to anxiety in patients with anorexia nervosa.

  15. Mass-controlled capillary viscometer for a Newtonian liquid: Viscosity of water at different temperatures

    Science.gov (United States)

    Digilov, Rafael M.; Reiner, M.

    2007-03-01

    The operation principle of the mass-controlled capillary viscometer is presented for a Newtonian liquid. The derived equation for the temporal changes of the mass in a liquid column draining under gravity through a discharge capillary tube accounts self-consistently for the inertial convective term associated with the acceleration effect. The viscosity of water measured at different temperatures using the new approach is in good agreement with literature data.

  16. An improved interface for capillary zone electrophoresis-mass spectrometry

    International Nuclear Information System (INIS)

    Smith, R.D.; Loo, J.A.; Barinaga, C.J.; Udseth, H.R.

    1988-06-01

    We have recently developed an improved electrospray ionization interface for capillary electrophoresis mass-spectrometry (CZE-MS). Our initial interface employed a vacuum deposited metal film at the exit of the capillary to make an electrical contact with he eluting buffer and establish the electrospray field gradient. This interface did, however, impose significant limitations on the range of capillary electrophoretic (CE) separations that could be performed. To circumvent these limitations, an interface that does not require a metalized tip was designed nd developed. In the new approach, the electrical contact at the column exit is made through a flowing liquid sheath. The principal advantage of this interface is that it allows operation with a much broader range of electrophoresis conditions. The sheath flow can be readily varied in both composition and volume. An electrospray ionization spectrum is given for a previously intractable buffer solution. 5 refs., 2 figs

  17. The Role of Non-Suicidal Self-Injury and Binge-Eating/Purging Behaviours in Family Functioning in Eating Disorders.

    Science.gov (United States)

    Depestele, Lies; Claes, Laurence; Dierckx, Eva; Baetens, Imke; Schoevaerts, Katrien; Lemmens, Gilbert M D

    2015-09-01

    This study aimed to investigate family functioning of restrictive and binge-eating/purging eating disordered adolescents with or without non-suicidal self-injury (NSSI), as perceived by the patients and their parents (mothers and fathers). In total, 123 patients (between 14 and 24 years), 98 mothers and 79 fathers completed the Family Assessment Device. Patients completed the Self-Injury Questionnaire-Treatment Related and the Symptom Checklist 90-Revised. No main effects were found of restrictive versus binge-eating/purging behaviour nor of presence/absence of NSSI. For the parents, a significant interaction between binge-eating/purging behaviour and NSSI emerged: Mothers and fathers reported worse family functioning in the binge-eating/purging group in presence of NSSI, whereas mothers reported worse family functioning in the restrictive group without NSSI. Parental perception of family functioning is affected by the combined presence of binge-eating/purging behaviour and NSSI. This finding should be taken into account when treating families living with eating disorders. Copyright © 2015 John Wiley & Sons, Ltd and Eating Disorders Association.

  18. Propellant and Purge System Contamination "2007: A Summer of Fun"

    Science.gov (United States)

    Galloway, Randy

    2010-01-01

    This slide presentation reviews the propellant and purge system contamination that occurred during the summer of 2007 at Stennis Space Center. During this period Multiple propellant/pressurant system contamination events prompted a thorough investigation, the results of which are reviewed.

  19. Human Reliability Analysis for In-Tank Precipitation Alignment and Startup of Emergency Purge Ventilation Equipment. Revision 3

    International Nuclear Information System (INIS)

    Shapiro, B.J.; Britt, T.E.

    1994-10-01

    This report documents the methodology used for calculating the human error probability for establishing air based ventilation using emergency purge ventilation equipment on In-Tank Precipitation (ITP) processing tanks 48 and 49 after failure of the nitrogen purge system following a seismic event. The analyses were performed according to THERP (Technique for Human Error Rate Prediction) as described in NUREG/CR-1278-F, ''Handbook of Human Reliability Analysis with Emphasis on Nuclear Power Plant Applications.'' The calculated human error probabilities are provided as input to the Fault Tree Analysis for the ITP Nitrogen Purge System

  20. Admittance Scanning for Whole Column Detection.

    Science.gov (United States)

    Stamos, Brian N; Dasgupta, Purnendu K; Ohira, Shin-Ichi

    2017-07-05

    Whole column detection (WCD) is as old as chromatography itself. WCD requires an ability to interrogate column contents from the outside. Other than the obvious case of optical detection through a transparent column, admittance (often termed contactless conductance) measurements can also sense changes in the column contents (especially ionic content) from the outside without galvanic contact with the solution. We propose here electromechanically scanned admittance imaging and apply this to open tubular (OT) chromatography. The detector scans across the column; the length resolution depends on the scanning velocity and the data acquisition frequency, ultimately limited by the physical step resolution (40 μm in the present setup). Precision equal to this step resolution was observed for locating an interface between two immiscible liquids inside a 21 μm capillary. Mechanically, the maximum scanning speed was 100 mm/s, but at 1 kHz sampling rate and a time constant of 25 ms, the highest practical scan speed (no peak distortion) was 28 mm/s. At scanning speeds of 0, 4, and 28 mm/s, the S/N for 180 pL (zone length of 1.9 mm in a 11 μm i.d. column) of 500 μM KCl injected into water was 6450, 3850, and 1500, respectively. To facilitate constant and reproducible contact with the column regardless of minor variations in outer diameter, a double quadrupole electrode system was developed. Columns of significant length (>1 m) can be readily scanned. We demonstrate its applicability with both OT and commercial packed columns and explore uniformity of retention along a column, increasing S/N by stopped-flow repeat scans, etc. as unique applications.

  1. JGOFS IV. Subproject: natural radionuclides as tracers for particle dynamics in the water column. Final report

    International Nuclear Information System (INIS)

    Scholten, J.C.; Fietzke, J.; Mangini, A.; Stoffers, P.

    2000-01-01

    As part of the German JOINT GLOBAL OCEAN FLUX STUDY (JGOFS) the aim of the project was to investigate the particle dynamics in the water column, especially to estimate the trapping efficiencies of sediment traps deployed in the eastern North Atlantic (L1: 33 N 21 W; L2: 47 N 19.5 W; L3: 54,4 N 21,1 W; ESTOC: 29,07 N 15,25 W; OMEX: 49 N 12,5 W). This investigation was based on measurements of the distribution of natural radionuclides in the water column and in sediment traps. In the upper water column (≤1000 m) the 230 Th concentrations are similar at all locations investigated and a reversible scavenging model was able to describe the 230 Th distribution. In the deep water-column at L2 and L3 the 230 Th concentrations were significantly lower than predicted from the reversible scavenging model. The 230 Th concentrations here could be described by a scavenging-mixing model which assumes an advection of 230 Th depleted water masses and a rapid ventilation between 3 and 25 years. Based on two models, a mass balance for 230 Th and 231 Pa and a constant removal model, sediment trap efficiencies were calculated to be between 9% and 143%. The lowest efficiencies (9%-36%) were determined in the 500 m and 1000 m traps and no direct relation between water currents velocities and trapping biases were observed. The correction for trapping biases were found to be important for the understanding of the regional differences in the particle flux in the eastern north Atlantic. (orig.) [de

  2. Evaluation of Purging Solutions for Military Fuel Tanks

    National Research Council Canada - National Science Library

    Rhee, In-Sik

    2003-01-01

    .... It is also a biodegradable water based solvent. Because of this property, US Army has used this environmentally friendly solvent as a purging solution in all military fuel tanks including Heavy Expanded Mobility Truck (HEMTT...

  3. Hydrogen recovery by pressure swing adsorption. [From ammonia purge-gas streams

    Energy Technology Data Exchange (ETDEWEB)

    1979-06-01

    A pressure swing absorption process (PSA) designed to recover H/sub 2/ from ammonia purge-gas streams developed by Bergbarr-Forschung GmbH of West Germany is reviewed. The PSA unit is installed in the process stream after the ammonia absorber unit which washes the ammonia-containing purge gas which consists of NH/sub 3/, H/sub 2/O, CH/sub 4/, Ar, N/sub 2/, and H/sub 2/. Usually 4 absorber units containing carbon molecular sieves make up the PSA unit; however, only one unit is generally used to absorb all components except H/sub 2/ while the other units are being regenerated by depressurization. Economic comparisons of the PSA process with a cryogenic process indicate that for some ammonia plants there may be a 30% saving in fuel gas requirements with the PSA system. The conditions of the purge gas strongly influence which system of recovery is more suitable.

  4. Colonic diverticular bleeding: urgent colonoscopy without purging and endoscopic treatment with epinephrine and hemoclips

    Directory of Open Access Journals (Sweden)

    Ignacio Couto-Worner

    2013-09-01

    Full Text Available Diverticular disease is the most frequent cause of lower gastrointestinal bleeding. Most of the times, bleeding stops without any intervention but in 10-20 % of the cases it is necessary to treat the hemorrhage. Several modalities of endoscopic treatment have been described after purging the colon. We present five cases of severe diverticular bleeding treated with injection of epinephrine and hemoclips. All the colonoscopies were performed without purging of the colon in an emergency setting, with correct visualization of the point of bleeding. Patients recovered well avoiding other aggressive procedures such as angiography or surgery.

  5. Catalytic membrane reactor for tritium extraction system from He purge

    International Nuclear Information System (INIS)

    Santucci, Alessia; Incelli, Marco; Sansovini, Mirko; Tosti, Silvano

    2016-01-01

    Highlights: • In the HCBB blanket, the produced tritium is recovered by purging with helium; membrane technologies are able to separate tritium from helium. • The paper presents the results of two experimental campaigns. • In the first, a Pd–Ag diffuser for hydrogen separation is tested at several operating conditions. • In the second, the ability of a Pd–Ag membrane reactor for water decontamination is assessed by performing isotopic swamping and water gas shift reactions. - Abstract: In the Helium Cooled Pebble Bed (HCPB) blanket concept, the produced tritium is recovered purging the breeder with helium at low pressure, thus a tritium extraction system (TES) is foreseen to separate the produced tritium (which contains impurities like water) from the helium gas purge. Several R&D activities are running in parallel to experimentally identify most promising TES technologies: particularly, Pd-based membrane reactors (MR) are under investigation because of their large hydrogen selectivity, continuous operation capability, reliability and compactness. The construction and operation under DEMO relevant conditions (that presently foresee a He purge flow rate of about 10,000 Nm 3 /h and a H 2 /He ratio of 0.1%) of a medium scale MR is scheduled for next year, while presently preliminary experiments on a small scale reactor are performed to identify most suitable operative conditions and catalyst materials. This work presents the results of an experimental campaign carried out on a Pd-based membrane aimed at measuring the capability of this device in separating hydrogen from the helium. Many operative conditions have been investigated by considering different He/H 2 feed flow ratios, several lumen pressures and reactor temperatures. Moreover, the performances of a membrane reactor (composed of a Pd–Ag tube having a wall thickness of about 113 μm, length 500 mm and diameter 10 mm) in processing the water contained in the purge gas have been measured by using

  6. Catalytic membrane reactor for tritium extraction system from He purge

    Energy Technology Data Exchange (ETDEWEB)

    Santucci, Alessia, E-mail: alessia.santucci@enea.it [ENEA for EUROfusion, Via E. Fermi 45, 00044 Frascati, Roma (Italy); Incelli, Marco [ENEA for EUROfusion, Via E. Fermi 45, 00044 Frascati, Roma (Italy); DEIM, University of Tuscia, Via del Paradiso 47, 01100 Viterbo (Italy); Sansovini, Mirko; Tosti, Silvano [ENEA for EUROfusion, Via E. Fermi 45, 00044 Frascati, Roma (Italy)

    2016-11-01

    Highlights: • In the HCBB blanket, the produced tritium is recovered by purging with helium; membrane technologies are able to separate tritium from helium. • The paper presents the results of two experimental campaigns. • In the first, a Pd–Ag diffuser for hydrogen separation is tested at several operating conditions. • In the second, the ability of a Pd–Ag membrane reactor for water decontamination is assessed by performing isotopic swamping and water gas shift reactions. - Abstract: In the Helium Cooled Pebble Bed (HCPB) blanket concept, the produced tritium is recovered purging the breeder with helium at low pressure, thus a tritium extraction system (TES) is foreseen to separate the produced tritium (which contains impurities like water) from the helium gas purge. Several R&D activities are running in parallel to experimentally identify most promising TES technologies: particularly, Pd-based membrane reactors (MR) are under investigation because of their large hydrogen selectivity, continuous operation capability, reliability and compactness. The construction and operation under DEMO relevant conditions (that presently foresee a He purge flow rate of about 10,000 Nm{sup 3}/h and a H{sub 2}/He ratio of 0.1%) of a medium scale MR is scheduled for next year, while presently preliminary experiments on a small scale reactor are performed to identify most suitable operative conditions and catalyst materials. This work presents the results of an experimental campaign carried out on a Pd-based membrane aimed at measuring the capability of this device in separating hydrogen from the helium. Many operative conditions have been investigated by considering different He/H{sub 2} feed flow ratios, several lumen pressures and reactor temperatures. Moreover, the performances of a membrane reactor (composed of a Pd–Ag tube having a wall thickness of about 113 μm, length 500 mm and diameter 10 mm) in processing the water contained in the purge gas have been

  7. Determination of DDTs and PCBs by capillary gas chromatography and electron capture detection

    International Nuclear Information System (INIS)

    1988-01-01

    This reference method deals with the determination of DDTs and PCBs in marine environmental samples using high resolution gas chromatography. Several other halogenated pesticides and other electron capturing organic compounds may be present in samples and many of these may also be determined by this method. Not all electron capturing residues will be resistant to all of the clean up procedures described here for the analysis of DTTs and PCBs. Therefore, additional information on the stability of some common pesticides using this methodology is also provided. The high separation power of open tubular (''capillary'') columns allows the identification and quantification of many compounds in the complex mixtures occurring in environmental samples. This manual provides information on the theoretical and practical aspects of the use of these high resolution columns for the analysis of DDTs and PCBs in environmental samples. The qualitative and quantitative method can be applied to any sample type (aerosol/vapour, water, particulates, biota, etc.) provided that suitable cleaned-up extracts dissolved in n-hexane are available for injection into the GC system. For example, methods for obtaining these cleaned-up sample extracts from marine organisms are described in detail in UNEP Reference Method no. 14 and for sediments in No. 17. The change in the field of application by analysing by capillary rather than packed columns may be less dramatic for DDTs. However, with the increased separation, the possibilities of inaccurate analysis resulting from overlap with interfering compounds is reduced. 7 refs, 1 fig., 3 tabs

  8. Purging sensitive science instruments with nitrogen in the STS environment

    Science.gov (United States)

    Lumsden, J. M.; Noel, M. B.

    1983-01-01

    Potential contamination of extremely sensitive science instruments during prelaunch, launch, and earth orbit operations are a major concern to the Galileo and International Solar Polar Mission (ISPM) Programs. The Galileo Program is developing a system to purify Shuttle supplied nitrogen gas for in-flight purging of seven imaging and non-imaging science instruments. Monolayers of contamination deposited on critical surfaces can degrade some instrument sensitivities as much as fifty percent. The purging system provides a reliable supply of filtered and fried nitrogen gas during these critical phases of the mission when the contamination potential is highest. The Galileo and ISPM Programs are including the system as Airborne Support Equipment (ASE).

  9. Disturbance of gut satiety peptide in purging disorder.

    Science.gov (United States)

    Keel, Pamela K; Eckel, Lisa A; Hildebrandt, Britny A; Haedt-Matt, Alissa A; Appelbaum, Jonathan; Jimerson, David C

    2018-01-01

    Little is known about biological factors that contribute to purging after normal amounts of food-the central feature of purging disorder (PD). This study comes from a series of nested studies examining ingestive behaviors in bulimic syndromes and specifically evaluated the satiety peptide YY (PYY) and the hunger peptide ghrelin in women with PD (n = 25), bulimia nervosa-purging (BNp) (n = 26), and controls (n = 26). Based on distinct subjective responses to a fixed meal in PD (Keel, Wolfe, Liddle, DeYoung, & Jimerson, ), we tested whether postprandial PYY response was significantly greater and ghrelin levels significantly lower in women with PD compared to controls and women with BNp. Participants completed structured clinical interviews, self-report questionnaires, and laboratory assessments of gut peptide and subjective responses to a fixed meal. Women with PD demonstrated a significantly greater postprandial PYY response compared to women with BNp and controls, who did not differ significantly. PD women also endorsed significantly greater gastrointestinal distress, and PYY predicted gastrointestinal intestinal distress. Ghrelin levels were significantly greater in PD and BNp compared to controls, but did not differ significantly between eating disorders. Women with BNp endorsed significantly greater postprandial hunger, and ghrelin predicted hunger. PD is associated with a unique disturbance in PYY response. Findings contribute to growing evidence of physiological distinctions between PD and BNp. Future research should examine whether these distinctions account for differences in clinical presentation as this could inform the development of specific interventions for patients with PD. © 2017 Wiley Periodicals, Inc.

  10. Depth dependent microbial carbon use efficiency in the capillary fringe as affected by water table fluctuations in a column incubation experiment

    Science.gov (United States)

    Pronk, G. J.; Mellage, A.; Milojevic, T.; Smeaton, C. M.; Rezanezhad, F.; Van Cappellen, P.

    2017-12-01

    Microbial growth and turnover of soil organic carbon (SOC) depend on the availability of electron donors and acceptors. The steep geochemical gradients in the capillary fringe between the saturated and unsaturated zones provide hotspots of soil microbial activity. Water table fluctuations and the associated drying and wetting cycles within these zones have been observed to lead to enhanced turnover of SOC and adaptation of the local microbial communities. To improve our understanding of SOC degradation under changing moisture conditions, we carried out an automated soil column experiment with integrated of hydro-bio-geophysical monitoring under both constant and oscillating water table conditions. An artificial soil mixture composed of quartz sand, montmorillonite, goethite and humus was used to provide a well-defined system. This material was inoculated with a microbial community extracted from a forested riparian zone. The soils were packed into 6 columns (60 cm length and 7.5 cm inner diameter) to a height of 45 cm; and three replicate columns were incubated under constant water table while another three were saturated and drained monthly. The initial soil development, carbon cycling and microbial community development were then characterized during 10 months of incubation. This system provides an ideal artificial gradient from the saturated to the unsaturated zone to study soil development from initially homogeneous materials and the same microbial community composition under controlled conditions. Depth profiles of SOC and microbial biomass after 329 days of incubation showed a depletion of carbon in the transition drying and wetting zone that was not associated with higher accumulation of microbial biomass, indicating a lower carbon use efficiency of the microbial community established within the water table fluctuation zone. This was supported by a higher ATP to microbial biomass carbon ratio within the same zone. The findings from this study highlight the

  11. Driven exercise in the absence of binge eating: Implications for purging disorder.

    Science.gov (United States)

    Lydecker, Janet A; Shea, Megan; Grilo, Carlos M

    2018-02-01

    Purging disorder (PD) is characterized by recurrent purging without objectively large binge-eating episodes. PD has received relatively little attention, and questions remain about the clinical significance of "purging" by exercise that is driven or compulsive (i.e., as extreme compensatory or weight-control behavior). The little available research suggests that individuals who use exercise as a compensatory behavior might have less eating-disorder psychopathology than those who purge by vomiting or laxatives, but those studies have had smaller sample sizes, defined PD using low-frequency thresholds, and defined exercise without weight-compensatory or driven elements. Participants (N = 2,017) completed a web-based survey with established measures of eating-disorder psychopathology, depression, and physical activity. Participants were categorized (regular compensatory driven exercise, PD-E, n = 297; regular compensatory vomiting/laxatives, PD-VL, n = 59; broadly defined anorexia nervosa, AN, n = 20; and no eating-disordered behaviors, NED, n = 1,658) and compared. PD-E, PD-VL, and AN had higher eating-disorder psychopathology and physical activity than NED but did not significantly differ from each other on most domains. PD-VL and AN had higher depression than PD-E, which was higher than NED. Findings suggest that among participants with regularly compensatory behaviors without binge eating, those who use exercise alone have similar levels of associated eating-disorder psychopathology as those who use vomiting/laxatives, although they have lower depression levels and overall frequency of purging. Findings provide further support for the clinical significance of PD. Clinicians and researchers should recognize the severity of driven exercise as a compensatory behavior, and the need for further epidemiological and treatment research. © 2017 Wiley Periodicals, Inc.

  12. Two-dimensional capillary electrophoresis: capillary isoelectric focusing and capillary zone electrophoresis with laser-induced fluorescence detection

    Science.gov (United States)

    Dickerson, Jane A.; Ramsay, Lauren M.; Dada, Oluwatosin O.; Cermak, Nathan

    2011-01-01

    Capillary isoelectric focusing and capillary zone electrophoresis are coupled with laser-induced fluorescence detection to create an ultrasensitive two-dimensional separation method for proteins. In this method, two capillaries are joined through a buffer filled interface. Separate power supplies control the potential at the injection end of the first capillary and at the interface; the detector is held at ground potential. Proteins are labeled with the fluorogenic reagent Chromeo P503, which preserves the isoelectric point of the labeled protein. The labeled proteins were mixed with ampholytes and injected into the first dimension capillary. A focusing step was performed with the injection end of the capillary at high pH and the interface at low pH. To mobilize components, the interface was filled with a high pH buffer, which was compatible with the second dimension separation. A fraction was transferred to the second dimension capillary for separation. The process of fraction transfer and second dimension separation was repeated two dozen times. The separation produced a spot capacity of 125. PMID:20603830

  13. Lamotrigine use in patients with binge eating and purging, significant affect dysregulation, and poor impulse control.

    Science.gov (United States)

    Trunko, Mary Ellen; Schwartz, Terry A; Marzola, Enrica; Klein, Angela S; Kaye, Walter H

    2014-04-01

    Some patients with symptoms of binge eating and purging are successfully treated with specific serotonin reuptake inhibitors (SSRIs), but others experience only partial or no benefit. Significant affect dysregulation and poor impulse control may be characteristics that limit responsiveness. We report on the treatment of five patients with bulimia nervosa (BN), anorexia nervosa-binge/purge type (AN-B/P) or eating disorder not otherwise specified (EDNOS), using the anticonvulsant lamotrigine after inadequate response to SSRIs. Following addition of lamotrigine to an antidepressant in four cases, and switch from an antidepressant to lamotrigine in one case, patients experienced substantial improvement in mood reactivity and instability, impulsive drives and behaviors, and eating-disordered symptoms. These findings raise the possibility that lamotrigine, either as monotherapy or as an augmenting agent to antidepressants, may be useful in patients who binge eat and purge, and have significant affect dysregulation with poor impulse control. Copyright © 2013 Wiley Periodicals, Inc.

  14. Cold Vacuum Drying (CVD) Facility Vacuum Purge System Chilled Water System Design Description. System 47-4

    International Nuclear Information System (INIS)

    IRWIN, J.J.

    2000-01-01

    This system design description (SDD) addresses the Vacuum Purge System Chilled Water (VPSCHW) system. The discussion that follows is limited to the VPSCHW system and its interfaces with associated systems. The reader's attention is directed to Drawings H-1-82162, Cold Vacuum Drying Facility Process Equipment Skid PandID Vacuum System, and H-1-82224, Cold Vacuum Drying Facility Mechanical Utilities Process Chilled Water PandID. Figure 1-1 shows the location and equipment arrangement for the VPSCHW system. The VPSCHW system provides chilled water to the Vacuum Purge System (VPS). The chilled water provides the ability to condense water from the multi-canister overpack (MCO) outlet gases during the MCO vacuum and purge cycles. By condensing water from the MCO purge gas, the VPS can assist in drying the contents of the MCO

  15. Preparation of polymer monolithic column functionalized by arsonic acid groups for mixed-mode capillary liquid chromatography.

    Science.gov (United States)

    Qin, Zhang-Na; Yu, Qiong-Wei; Wang, Ren-Qi; Feng, Yu-Qi

    2018-04-27

    A mixed-mode polymer monolithic column functionalized by arsonic acid groups was prepared by single-step in situ copolymerization of monomers p-methacryloylaminophenylarsonic acid (p-MAPHA) and pentaerythritol triacrylate (PETA). The prepared poly(p-MAPHA-co-PETA) monolithic column has a homogeneous monolithic structure with good permeability and mechanical stability. Zeta potential measurements reveal that the monolithic stationary phase holds a negative surface charge when the mobile phase resides in the pH range of 3.0-8.0. The retention mechanisms of prepared monolithic column are explored by the separation of selected polycyclic aromatic hydrocarbons (PAHs), nucleosides, and three basic compounds. The results indicate that the column functions in three different separation modes associated with reversed-phase chromatography based on hydrophobic interaction, hydrophilic interaction chromatography, and cation-exchange chromatography. The column efficiency of prepared monolithic column is estimated to be 70,000 and 76,000 theoretical plates/m for thiourea and naphthalene, respectively, at a linear flow velocity of 0.85 mm/s using acetonitrile/H 2 O (85/15, v/v) as the mobile phase. Furthermore, an analysis of the retention factors obtained for the PAHs indicates that the prepared monolithic column exhibits good reproducibility with relative standard deviations of 2.9%, 4.0%, and 4.7% based on run-to-run injections, column-to-column preparation, and batch-to-batch preparation, respectively. Finally, we investigate the separation performance of the proposed monolithic column for select phenols, sulfonamides, nucleobases and nucleosides. Copyright © 2018 Elsevier B.V. All rights reserved.

  16. On-line combination of liquid chromatography and capillary gas chromatography : preconcentration and analysis of organic compounds in aqueous samples

    NARCIS (Netherlands)

    Noij, T.H.M.; Weiss, E.; Herps, T.; Cruchten, van H.; Rijks, J.A.

    1988-01-01

    This paper describes the design of a new, versatile, and low-cost on-line LC-GC interface that allows the fast and reliable introduction of large sample volumes onto a capillary GC column. The sample introduction procedure consists successively of: evaporation of the entire sample (LC fraction),

  17. Appetite Regulatory Hormones in Women With Anorexia Nervosa: Binge-Eating/Purging Versus Restricting Type

    Science.gov (United States)

    Eddy, Kamryn T.; Lawson, Elizabeth A.; Meade, Christina; Meenaghan, Erinne; Horton, Sarah E.; Misra, Madhusmita; Klibanski, Anne; Miller, Karen K.

    2015-01-01

    Objective Anorexia nervosa is a psychiatric illness characterized by low weight, disordered eating, and hallmark neuroendocrine dysfunction. Behavioral phenotypes are defined by predominant restriction or bingeing/purging; binge-eating/purging type anorexia nervosa is associated with poorer outcome. The pathophysiology underlying anorexia nervosa types is unknown, but altered hormones, known to be involved in eating behaviors, may play a role. Method To examine the role of anorexigenic hormones in anorexia nervosa subtypes, we examined serum levels of peptide YY (PYY; total and active [3-36] forms), brain-derived neurotrophic factor (BDNF), and leptin as primary outcomes in women with OSM-5 restricting type anorexia nervosa (n=50), binge-eating/purging type anorexia nervosa (n = 22), and healthy controls (n = 22).1n addition, women completed validated secondary outcome measures of eating disorder psychopathology (Eating Disorder Examination-Questionnaire) and depression and anxiety symptoms (Hamilton Rating Scales for Depression [HDRS] and Anxiety [HARS]). The study samples were collected from May 22, 2004, to February 7, 2012. Results Mean PYY 3-36 and leptin levels were lower and BDNF levels higher in binge-eating/purging type anorexia nervosa than in restricting type anorexia nervosa (all Pvalues anorexia nervosa types were significant (Panorexia nervosa, the anorexigenic hormones PYY, BDNF, and leptin are differentially regulated between the restricting and binge/purge types. Whether these hormone pathways play etiologic roles with regard to anorexia nervosa behavioral types or are compensatory merits further study. PMID:25098834

  18. Residual CO2 trapping in Indiana limestone.

    Science.gov (United States)

    El-Maghraby, Rehab M; Blunt, Martin J

    2013-01-02

    We performed core flooding experiments on Indiana limestone using the porous plate method to measure the amount of trapped CO(2) at a temperature of 50 °C and two pressures: 4.2 and 9 MPa. Brine was mixed with CO(2) for equilibration, then the mixture was circulated through a sacrificial core. Porosity and permeability tests conducted before and after 884 h of continuous core flooding confirmed negligible dissolution. A trapping curve for supercritical (sc)CO(2) in Indiana showing the relationship between the initial and residual CO(2) saturations was measured and compared with that of gaseous CO(2). The results were also compared with scCO(2) trapping in Berea sandstone at the same conditions. A scCO(2) residual trapping end point of 23.7% was observed, indicating slightly less trapping of scCO(2) in Indiana carbonates than in Berea sandstone. There is less trapping for gaseous CO(2) (end point of 18.8%). The system appears to be more water-wet under scCO(2) conditions, which is different from the trend observed in Berea; we hypothesize that this is due to the greater concentration of Ca(2+) in brine at higher pressure. Our work indicates that capillary trapping could contribute to the immobilization of CO(2) in carbonate aquifers.

  19. Static Response of Microbeams due to Capillary and Electrostatic Forces

    KAUST Repository

    Bataineh, Ahmad M.

    2016-03-07

    Micro-sensors or micro-switches usually operate under the effect of electrostatic force and could face some environmental effects like humidity, which may lead to condensation underneath the beams and create strong capillary forces. Those tiny structures are principally made of microbeams that can undergo instabilities under the effect of those created huge capillary forces. In fact, during the fabrication of microbeams, there is an important step to separate the beam from its substrate (wet etching). After this step, the microstructure is dried, which may causes the onset of some droplets of water trapped underneath the beam that could bring about a huge capillary force pulling it toward its substrate. If this force is bigger than the microbeam\\'s restoring force, it will become stuck to the substrate. This paper investigates the instability scenarios of both clamped-clamped (straight and curved) and cantilever (straight and curled) microbeams under the effect of capillary and/or electrostatic forces. The reduced order modeling (ROM) based on the Galerkin procedure is used to solve the nonlinear beam equations. The non-ideal boundaries are modeled by adding springs. The volume of the fluid between the beam and the substrate underneath it is varied and the relation between the volume of the water and the stability of the beam is shown. An analysis for the factors of which should be taken in to consideration in the fabrication processes to overcome the instability due to huge capillary forces is done. Also the size of the electrode for the electrostatic force is varied to show the effect on the micro-switch stability. A variation of the pull-in voltage with some specific beam parameters and with more than one case of electrode size is shown. It is found that capillary forces have a pronounced effect on the stability of microbeams. It is also found that the pull-in length decreases as the electrode size increases. It is also shown that the pull-in voltage decreases

  20. Poly(norepinephrine)-coated open tubular column for the separation of proteins and recombination human erythropoietin by capillary electrochromatography.

    Science.gov (United States)

    Xiao, Xue; Zhang, Yamin; Wu, Jia; Jia, Li

    2017-12-01

    Recombinant human erythropoietin is an important therapeutic protein with high economic interest due to the benefits provided by its clinical use for the treatment of anemias associated with chronic renal failure and chemotherapy. In this work, a poly(norepinephrine)-coated open tubular column was successfully prepared based on the self-polymerization of norepinephrine under mild alkaline condition, the favorable film forming and easy adhesive properties of poly(norepinephrine). The poly(norepinephrine) coating was characterized by scanning electron microscopy and measurement of the electro-osmotic flow. The thickness of the coating was about 431 nm. The electrochromatographic performance of the poly(norepinephrine)-coated open tubular column was evaluated by separation of proteins. Some basic and acidic proteins including two variants of bovine serum albumin and two variants of β-lactoglobulin achieved separation in the poly(norepinephrine)-coated open tubular column. More importantly, the column demonstrated separation ability for the glycoforms of recombinant human erythropoietin. In addition, the column demonstrated good repeatability with the run-to-run, day-to-day, and column-to-column relative standard deviations of migration times of proteins less than 3.40%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Slope wavenumber spectrum models of capillary and capillary-gravity waves

    Institute of Scientific and Technical Information of China (English)

    贾永君; 张杰; 王岩峰

    2010-01-01

    Capillary and capillary-gravity waves possess a random character, and the slope wavenumber spectra of them can be used to represent mean distributions of wave energy with respect to spatial scale of variability. But simple and practical models of the slope wavenumber spectra have not been put forward so far. In this article, we address the accurate definition of the slope wavenumber spectra of water surface capillary and capillary-gravity waves. By combining the existing slope wavenumber models and using th...

  2. The dynamic behavior of pressure during purge process in the anode of a PEM fuel cell

    Energy Technology Data Exchange (ETDEWEB)

    Gou, Jun; Pei, Pucheng; Wang, Ying [State Key Laboratory of Automotive Safety and Energy, Tsinghua University, Beijing 100084 (China)

    2006-11-22

    A one-dimensional mathematic computational fluid dynamics model of a proton exchange membrane (PEM) fuel cell is presented in this paper to simulate the transient behavior of hydrogen pressure in the flow field during a typical dynamic process-the purge process. This model accounts for the mechanism of pressure wave transmission in the channels by employing the characteristic line method. A unique parameter-pressure swing, which represents the top value of pressure variation at certain point in the channel during the purge process, is brought up and studied as well as the pressure drop. The pressure distribution along the channel and the pressure drop during the purge process for different operating pressures, lengths of purge time, stoichiometric ratios and current densities are studied. The results indicate that the distributed pressure, pressure drop and pressure swing all increase with the increment of operating pressure. With a high operating pressure a second-falling stage can be seen in the pressure drop profile while with a relatively low operating pressure, a homogeneous distribution of pressure swing can be attained. A long purge time will provide enough time to show the whole part of the pressure drop curve, while only a part of the curve can be attained if a short purge time is adopted, but a relatively uniform distribution of pressure swing will show up at the moment. Compared with the condition of stoichiometric ratio 1, the pressure drop curve decreases more sharply after the top value and the pressure swing displays a more uniform distribution when the ratio is set beyond 1. Different current densities have no apparent influence on the pressure drop and the pressure swing during this transient process. All the distribution rules of related parameters deducted from this study will be helpful for optimizing the purging strategies on vehicles. (author)

  3. Cardiac Risk and Disordered Eating: Decreased R Wave Amplitude in Women with Bulimia Nervosa and Women with Subclinical Binge/Purge Symptoms.

    Science.gov (United States)

    Green, Melinda; Rogers, Jennifer; Nguyen, Christine; Blasko, Katherine; Martin, Amanda; Hudson, Dominique; Fernandez-Kong, Kristen; Kaza-Amlak, Zauditu; Thimmesch, Brandon; Thorne, Tyler

    2016-11-01

    The purpose of the present study was threefold. First, we examined whether women with bulimia nervosa (n = 12) and women with subthreshold binge/purge symptoms (n = 20) showed decreased mean R wave amplitude, an indicator of cardiac risk, on electrocardiograph compared to asymptomatic women (n = 20). Second, we examined whether this marker was pervasive across experimental paradigms, including before and after sympathetic challenge tasks. Third, we investigated behavioural predictors of this marker, including binge frequency and purge frequency assessed by subtype (dietary restriction, excessive exercise, self-induced vomiting, and laxative abuse). Results of a 3 (ED symptom status) × 5 (experimental condition) mixed factorial ANCOVA (covariates: body mass index, age) indicated women with bulimia nervosa and women with subclinical binge/purge symptoms demonstrated significantly reduced mean R wave amplitude compared to asymptomatic women; this effect was pervasive across experimental conditions. Multiple regression analyses showed binge and purge behaviours, most notably laxative abuse as a purge method, predicted decreased R wave amplitude across all experimental conditions. Copyright © 2016 John Wiley & Sons, Ltd and Eating Disorders Association. Copyright © 2016 John Wiley & Sons, Ltd and Eating Disorders Association.

  4. Supercritical fluid extraction-capillary gas chromatography: on-line coupling with a programmed temperature vaporizer

    NARCIS (Netherlands)

    Houben, R.J.; Janssen, J.G.M.; Leclercq, P.A.; Rijks, J.A.; Cramers, C.A.M.G.

    1990-01-01

    A simple and versatile system is described for the on-line coupling of SFE to capillary GC. The interfacing consists of a programmed temperature vaporizer (PTV) injector. With this injector it is possible to combine solute trapping, elimination of a high flow of extraction fluid, and quantitative

  5. Mixed Fluid Conditions: Capillary Phenomena

    KAUST Repository

    Santamarina, Carlos

    2017-07-06

    Mixed fluid phenomena in porous media have profound implications on soil-atmosphere interaction, energy geotechnology, environmental engineering and infrastructure design. Surface tension varies with pressure, temperature, solute concentration, and surfactant concentration; on the other hand, the contact angle responds to interfacial tensions, surface topography, invasion velocity, and chemical interactions. Interfaces are not isolated but interact through the fluid pressure and respond to external fields. Jumps, snap-offs and percolating wetting liquids along edges and crevices are ubiquitous in real, non-cylindrical porous networks. Pore- and macroscale instabilities together with pore structure variability-and-correlation favor fluid trapping and hinder recovery efficiency. The saturation-pressure characteristic curve is affected by the saturation-history, flow-rate, the mechanical response of the porous medium, and time-dependent reactive and diffusive processes; in addition, there are salient differences between unsaturation by internal gas nucleation and gas invasion. Capillary forces add to other skeletal forces in the porous medium and can generate open-mode discontinuities when the capillary entry pressure is high relative to the effective stress. Time emerges as an important variable in mixed-fluid conditions and common quasi-static analyses may fail to capture the system response.

  6. Better Fitness in Captive Cuvier's Gazelle despite Inbreeding Increase: Evidence of Purging?

    Directory of Open Access Journals (Sweden)

    Eulalia Moreno

    Full Text Available Captive breeding of endangered species often aims at preserving genetic diversity and to avoid the harmful effects of inbreeding. However, deleterious alleles causing inbreeding depression can be purged when inbreeding persists over several generations. Despite its great importance both for evolutionary biology and for captive breeding programmes, few studies have addressed whether and to which extent purging may occur. Here we undertake a longitudinal study with the largest captive population of Cuvier's gazelle managed under a European Endangered Species Programme since 1975. Previous results in this population have shown that highly inbred mothers tend to produce more daughters, and this fact was used in 2006 to reach a more appropriate sex-ratio in this polygynous species by changing the pairing strategy (i.e., pairing some inbred females instead of keeping them as surplus individuals in the population. Here, by using studbook data we explore whether purging has occurred in the population by investigating whether after the change in pairing strategy a inbreeding and homozygosity increased at the population level, b fitness (survival increased, and c the relationship between inbreeding and juvenile survival, was positive. Consistent with the existence of purging, we found an increase in inbreeding coefficients, homozygosity and juvenile survival. In addition, we showed that in the course of the breeding programme the relationship between inbreeding and juvenile survival was not uniform but rather changed over time: it was negative in the early years, flat in the middle years and positive after the change in pairing strategy. We highlight that by allowing inbred individuals to mate in captive stocks we may favour sex-ratio bias towards females, a desirable managing strategy to reduce the surplus of males that force most zoos to use ethical culling and euthanizing management tools. We discuss these possibilities but also acknowledge that many

  7. Effect of the purging gas on properties of Ti stabilized AISI 321 stainless steel TIG welds

    Energy Technology Data Exchange (ETDEWEB)

    Taban, Emel; Kaluc, Erdinc; Aykan, T. Serkan [Kocaeli Univ. (Turkey). Dept. of Mechanical Engineering

    2014-07-01

    Gas purging is necessary to provide a high quality of stainless steel pipe welding in order to prevent oxidation of the weld zone inside the pipe. AISI 321 stabilized austenitic stainless steel pipes commonly preferred in refinery applications have been welded by the TIG welding process both with and without the use of purging gas. As purging gases, Ar, N{sub 2}, Ar + N{sub 2} and N{sub 2} + 10% H{sub 2} were used, respectively. The aim of this investigation is to detect the effect of purging gas on the weld joint properties such as microstructure, corrosion, strength and impact toughness. Macro sections and microstructures of the welds were investigated. Chemical composition analysis to obtain the nitrogen, oxygen and hydrogen content of the weld root was done by Leco analysis. Ferrite content of the beads including root and cap passes were measured by a ferritscope. Vickers hardness (HV10) values were obtained. Intergranular and pitting corrosion tests were applied to determine the corrosion resistance of all welds. Type of the purging gas affected pitting corrosion properties as well as the ferrite content and nitrogen, oxygen and hydrogen contents at the roots of the welds. Any hot cracking problems are not predicted as the weld still solidifies with ferrite in the primary phase as confirmed by microstructural and ferrite content analysis. Mechanical testing showed no significant change according to the purge gas. AISI 321 steel and 347 consumable compositions would permit use of nitrogen rich gases for root shielding without a risk of hot cracking.

  8. Human Reliability Analysis for In-Tank Precipitation Alignment and Startup of Emergency Purge Ventilation Equipment. Revision 4

    International Nuclear Information System (INIS)

    Shapiro, B.J.; Britt, T.E.

    1995-06-01

    This report documents the methodology used for calculating the human error probability for establishing air based ventilation using emergency purge ventilation equipment on In-Tank Precipitation (ITP) processing tanks 48 and 49 after a failure of the nitrogen purge system following a seismic event. The analyses were performed according to THERP (Technique for Human Error Rate Prediction) as describes in NUREG/CR-1278-F

  9. CEC-atmospheric pressure ionization MS of pesticides using a surfactant-bound monolithic column.

    Science.gov (United States)

    Gu, Congying; Shamsi, Shahab A

    2010-04-01

    A surfactant bound poly (11-acrylaminoundecanoic acid-ethylene dimethacrylate) monolithic column was simply prepared by in situ co-polymerization of 11-acrylaminoundecanoic acid and ethylene dimethacrylate with 1-propanol, 1,4-butanediol and water as porogens in 100 microm id fused-silica capillary in one step. This column was used in CEC-atmospheric pressure photoionization (APPI)-MS system for separation and detection of N-methylcarbamates pesticides. Numerous parameters are optimized for CEC-APPI-MS. After evaluation of the mobile phase composition, sheath liquid composition and the monolithic capillary outlet position, a fractional factorial design was selected as a screening procedure to identify factors of ionization source parameters, such as sheath liquid flow rate, drying gas flow rate, drying gas temperature, nebulizing gas pressure, vaporizer temperature and capillary voltage, which significantly influence APPI-MS sensitivity. A face-centered central composite design was further utilized to optimize the most significant parameters and predict the best sensitivity. Under optimized conditions, S/Ns around 78 were achieved for an injection of 100 ng/mL of each pesticide. Finally, this CEC-APPI-MS method was successfully applied to the analysis of nine N-methylcarbamates in spiked apple juice sample after solid phase extraction with recoveries in the range of 65-109%.

  10. Capillary electrophoretic study of individual exocytotic events in single mast cells

    Energy Technology Data Exchange (ETDEWEB)

    Ho, Andrea Ming-Wei [Iowa State Univ., Ames, IA (United States)

    1999-02-12

    The peak profile of individual degranulation events from the on-column release of serotonin from single rat peritoneal mast cells (RPMCs) was monitored using capillary electrophoresis with laser-induced native fluorescence detection (CE-LINF). Serotonin, an important biogenic amine, is contained in granules (0.25 fL) within RPMCs and is extruded by a process termed exocytosis. The secretagogue, Polymyxin B sulfate, was used as the CE running buffer after injection of a single RPMC into the separation capillary to stimulate the release of the granules. Because the release process occurs on a ms time scale, monitoring individual exocytotic events is possible with the coupling of high-speed CE and LINF detection.

  11. CO2-laser--produced plasma columns in a solenoidal magnetic field

    International Nuclear Information System (INIS)

    Offenberger, A.A.; Cervenan, M.R.; Smy, P.R.

    1976-01-01

    A 1-GW CO 2 laser pulse has been used to produce extended column breakdown of hydrogen at low pressure in a 20-cm-long solenoid. Magnetic fields of up to 110 kG were used to inhibit radial losses of the plasma column. A differential pumping scheme was devised to prevent formation of an opaque absorption wave travelling out of the solenoid back toward the focusing lens. Target burns give direct evidence for trapped laser beam propagation along the plasma column

  12. Coatings of molecularly imprinted polymers based on polyhedral oligomeric silsesquioxane for open tubular capillary electrochromatography.

    Science.gov (United States)

    Zhao, Qing-Li; Zhou, Jin; Zhang, Li-Shun; Huang, Yan-Ping; Liu, Zhao-Sheng

    2016-05-15

    Polyhedral oligomeric silsesquioxane (POSS) was successfully applied, for the first time, to prepare imprinted monolithic coating for capillary electrochromatography. The imprinted monolithic coating was synthesized with a mixture of PSS-(1-Propylmethacrylate)-heptaisobutyl substituted (MA 0702), S-amlodipine (template), methacrylic acid (functional monomer), and 2-methacrylamidopropyl methacrylate (crosslinker), in a porogenic mixture of toluene-isooctane. The influence of synthesis parameters on the imprinting effect and separation performance, including the amount of MA 0702, the ratio of template to monomer, and the ratio of monomer to crosslinker, was investigated. The greatest resolution for enantiomers separation on the imprinted monolithic column prepared with MA 0702 was up to 22.3, about 2 times higher than that prepared in absence of the POSS. Column efficiency on the POSS-based MIP coatings was beyond 30,000 plate m(-1). The comparisons between MIP coating synthesized with the POSS and without the POSS were made in terms of selectivity, column efficiency, and resolution. POSS-based MIP capillaries with naproxen or zopiclone was also prepared and separation of enantiomers can be achieved. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Computational fluid dynamic simulation of pressurizer safety valve loop seal purge phenomena in nuclear power plants

    International Nuclear Information System (INIS)

    Park, Jong Woon

    2012-01-01

    In Korean 3 Loop plants a water loop seal pipe is installed containing condensed water upstream of a pressurizer safety valve to protect the valve disk from the hot steam environment. The loop seal water purge time is a key parameter in safety analyses for overpressure transients, because it delays valve opening. The loop seal purge time is uncertain to measure by test and thus 3-dimensional realistic computational fluid dynamics (CFD) model is developed in this paper to predict the seal water purge time before full opening of the valve which is driven by steam after water purge. The CFD model for a typical pressurizer safety valve with a loop seal pipe is developed using the computer code of ANSYS CFX 11. Steady-state simulations are performed for full discharge of steam at the valve full opening. Transient simulations are performed for the loop seal dynamics and to estimate the loop seal purge time. A sudden pressure drop higher than 2,000 psia at the tip of the upper nozzle ring is expected from the steady-state calculation. Through the transient simulation, almost loop seal water is discharged within 1.2 second through the narrow opening between the disk and the nozzle of the valve. It can be expected that the valve fully opens at least before 1.2 second because constant valve opening is assumed in this CFX simulation, which is conservative because the valve opens fully before the loop seal water is completely discharged. The predicted loop seal purge time is compared with previous correlation. (orig.)

  14. Computational fluid dynamic simulation of pressurizer safety valve loop seal purge phenomena in nuclear power plants

    Energy Technology Data Exchange (ETDEWEB)

    Park, Jong Woon [Dongguk Univ., Gyeongju (Korea, Republic of). Nuclear and Energy Engineering Dept.

    2012-11-15

    In Korean 3 Loop plants a water loop seal pipe is installed containing condensed water upstream of a pressurizer safety valve to protect the valve disk from the hot steam environment. The loop seal water purge time is a key parameter in safety analyses for overpressure transients, because it delays valve opening. The loop seal purge time is uncertain to measure by test and thus 3-dimensional realistic computational fluid dynamics (CFD) model is developed in this paper to predict the seal water purge time before full opening of the valve which is driven by steam after water purge. The CFD model for a typical pressurizer safety valve with a loop seal pipe is developed using the computer code of ANSYS CFX 11. Steady-state simulations are performed for full discharge of steam at the valve full opening. Transient simulations are performed for the loop seal dynamics and to estimate the loop seal purge time. A sudden pressure drop higher than 2,000 psia at the tip of the upper nozzle ring is expected from the steady-state calculation. Through the transient simulation, almost loop seal water is discharged within 1.2 second through the narrow opening between the disk and the nozzle of the valve. It can be expected that the valve fully opens at least before 1.2 second because constant valve opening is assumed in this CFX simulation, which is conservative because the valve opens fully before the loop seal water is completely discharged. The predicted loop seal purge time is compared with previous correlation. (orig.)

  15. Determination of thromboxanes, leukotrienes and lipoxins using high-temperature capillary liquid chromatography-tandem mass spectrometry and on-line sample preparation

    DEFF Research Database (Denmark)

    Dahl, Sandra Rinne; Kleiveland, Charlotte Ramstad; Kassem, Moustapha

    2009-01-01

    An on-line strong cation-exchange (SCX)-reversed-phase (RP) capillary liquid chromatographic (cLC) method with ion-trap tandem mass spectrometric (IT-MS/MS) detection for the simultaneous determination of thromboxane (TX) B(2), TXB(3), leukotriene (LT) B(4), LTD(4) and lipoxin (LX) A(4) in cell...

  16. N2 vs H20 as purge/hydrostatic head

    International Nuclear Information System (INIS)

    Mast, J.C.

    1996-01-01

    This document provides the information to explain to the customer the ETP for the N2 vs H20 as Purge/Hydrostatic Head. This ETP follows the format described in Issurance of New Characterization Equipment Engineering Desk Instructions, 75200-95-013

  17. Direct measurement of lithium in whole blood using microchip capillary electrophoresis with integrated conductivity detection

    NARCIS (Netherlands)

    Vrouwe, E.X.; Lüttge, Regina; van den Berg, Albert

    2004-01-01

    The direct measurement of lithium in whole blood is described. Using microchip capillary electrophoresis (CE) with defined sample loading and applying the principles of column coupling, alkali metals were determined in a drop of whole blood. Blood collected from a finger stick was mixed with

  18. High sensitivity and selectivity in quantitative analysis of drugs in biological samples using 4-column multidimensional micro-UHPLC-MS enabling enhanced sample loading capacity.

    Science.gov (United States)

    de Vries, Ronald; Vereyken, Liesbeth; François, Isabelle; Dillen, Lieve; Vreeken, Rob J; Cuyckens, Filip

    2017-10-09

    Sensitivity is often a critical parameter in quantitative bioanalyses in drug development. For liquid-chromatography-based methods, sensitivity can be improved by reducing the column diameter, but practical sensitivity gains are limited by the reduced sample loading capacity on small internal diameter (I.D.) columns. We developed a set-up that has overcome these limitations in sample loading capacity. The set-up uses 4 columns with gradually decreasing column diameters along the flow-path (2.1 → 1 → 0.5 → 0.15 mm). Samples are pre-concentrated on-line on a 2.1 mm I.D. trapping column and back flushed to a 1 mm I.D. UHPLC analytical column and separated. The peak(s) of interest are transferred using heartcutting to a second trapping column (0.5 mm I.D.), which is back-flushed to a 0.15 mm I.D. micro-UHPLC analytical column for orthogonal separation. The proof of concept of the set-up was demonstrated by the simultaneous analysis of midazolam and 1'-hydroxy midazolam in plasma by injection of 80 μL of protein precipitated plasma. The 4-column funnel set-up proved to be robust and resulted in a 10-50 times better sensitivity compared to a trap-elute approach and 250-500 fold better compared to direct micro-UHPLC analysis. A lower limit of quantification of 100 fg/mL in plasma was obtained for both probe compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Characterizations of gas purge valves for liquid alignment and gas removal in a microfluidic chip

    International Nuclear Information System (INIS)

    Chuang, Han-Sheng; Thakur, Raviraj; Wereley, Steven T

    2012-01-01

    Two polydimethylsiloxane (PDMS) gas purge valves for excessive gas removal in general lab-on-a-chip applications are presented in this paper. Both valves are devised based on a three-layer configuration comprising a top layer for liquid channels, a membrane and a bottom layer for gas channels. The pneumatic valves work as a normal gateway for fluids when the membrane is bulged down (open state) by vacuum or pushed up (closed state) by pressure. In the closed state, the air in front of a liquid can be removed through a small notch or a permeable PDMS membrane by compressing the liquid. The purge valve with a small notch across its valve seat, termed surface-tension (ST) valve, can be operated with pressure under 11.5 kPa. The liquid is mainly retained by the surface tension resulting from the hydrophobic channel walls. In contrast, the purge valve with vacuum-filled grooves adjacent to a liquid channel, termed gas-permeation (GP) valve, can be operated at pressure above 5.5 kPa. Based on the principle of gas permeation, the excessive air can be slowly removed through the vent grooves. Detailed evaluations of both valves in a pneumatically driven microfluidic chip were conducted. Specifically, the purge valves enable users to remove gas and passively align liquids at desired locations without using sensing devices or feedback circuits. Finally, a rapid mixing reaction was successfully performed with the GP valves, showing their practicability as incorporated in a microfluidic chip. (paper)

  20. Microwave discharges in capillary tubes

    International Nuclear Information System (INIS)

    Dervisevic, Emil

    1984-01-01

    This research thesis aims at being a contribution to the study of microwave discharge by a surface wave, and more precisely focusses on the discharge in capillary tubes filled with argon. The author first present theoretical models which describe, on the one hand, the propagation of the surface wave along the plasma column, and, on the other hand, longitudinal and radial profiles of the main discharge characteristics. The second part addresses the study of the influence of parameters (gas pressure and tube radius) on discharge operation and characteristics. Laws of similitude as well as empirical relationships between argon I and argon II emission line intensities, electron density, and electric field in the plasma have been established [fr

  1. Jurin's law revisited: Exact meniscus shape and column height.

    Science.gov (United States)

    Liu, Sai; Li, Shanpeng; Liu, Jianlin

    2018-03-30

    Capillary rise of a liquid column is a historical problem, which has normally been formulated by Jurin's law. In the present study, we investigate the exact solutions of the column height, considering the real shape of the meniscus according to the Young-Laplace equation. The analytical solution in the planar model and the numerical solution in the axisymmetric model on the meniscus shape are both given, which are compared with the results from Jurin's law, modified Jurin's law and Surface Evolver simulation. The results quantitatively show that when the distance between the two plates or the diameter of the tube becomes bigger, Jurin's law and modified Jurin's law would cause serious errors, and the profile morphology of the meniscus must be calculated according to the Young-Laplace equation. These findings are beneficial for us to better understand the mechanism of capillarity and wetting, which are promising for such areas as oil displacement, ore floatation, building materials, fabrics, etc.

  2. Monitoring the behaviour of 4-ketocyclophosphamide versus cyclophosphamide during capillary gas chromatography by mass spectrometry

    NARCIS (Netherlands)

    Bruijn, de E.A.; Oosterom, van A.T.; Leclercq, P.A.; Haan, de J.W.; Ven, van de L.J.M.; Tjaden, U.R.

    1987-01-01

    Capillary Gas Chromatography (CGC) is capable of determining underivatized cyclophosphamide (CPA) using SCOT OV 275 columns. Then CPA is subjected to in situ degradation resulting in formation of a cyclization product which can be determined selectively in biological fluids. In routine bioanalysis

  3. Polar and nonpolar organic polymer-based monolithic columns for capillary electrochromatography and high-performance liquid chromatography.

    Science.gov (United States)

    Rathnasekara, Renuka; Khadka, Shantipriya; Jonnada, Murthy; El Rassi, Ziad

    2017-01-01

    This review article is a continuation of the previous reviews on the area of monolithic columns covering the progress made in the field over the last couple of years from the beginning of the second half of 2014 until the end of the first half of 2016. It summarizes and evaluates the evolvement of both polar and nonpolar organic monolithic columns and their use in hydrophilic interaction LC and CEC and reversed-phase chromatography and RP-CEC. The review article discusses the results reported in a total of 62 references. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Effect of Initial Hydraulic Conditions on Capillary Rise in a Porous Medium: Pore-Network Modeling

    KAUST Repository

    Joekar-Niasar, V.

    2012-01-01

    The dynamics of capillary rise in a porous medium have been mostly studied in initially dry systems. As initial saturation and initial hydraulic conditions in many natural and industrial porous media can be variable, it is important to investigate the influence of initial conditions on the dynamics of the process. In this study, using dynamic pore-network modeling, we simulated capillary rise in a porous medium for different initial saturations (and consequently initial capillary pressures). Furthermore, the effect of hydraulic connectivity of the wetting phase in corners on the height and velocity of the wetting front was studied. Our simulation results show that there is a trade-off between capillary forces and trapping due to snap-off, which leads to a nonlinear dependence of wetting front velocity on initial saturation at the pore scale. This analysis may provide a possible answer to the experimental observations in the literature showing a non-monotonic dependency between initial saturation and the macroscopic front velocity. © Soil Science Society of America.

  5. Effects of intermediate wettability on entry capillary pressure in angular pores.

    Science.gov (United States)

    Rabbani, Harris Sajjad; Joekar-Niasar, Vahid; Shokri, Nima

    2016-07-01

    Entry capillary pressure is one of the most important factors controlling drainage and remobilization of the capillary-trapped phases as it is the limiting factor against the two-phase displacement. It is known that the entry capillary pressure is rate dependent such that the inertia forces would enhance entry of the non-wetting phase into the pores. More importantly the entry capillary pressure is wettability dependent. However, while the movement of a meniscus into a strongly water-wet pore is well-defined, the invasion of a meniscus into a weak or intermediate water-wet pore especially in the case of angular pores is ambiguous. In this study using OpenFOAM software, high-resolution direct two-phase flow simulations of movement of a meniscus in a single capillary channel are performed. Interface dynamics in angular pores under drainage conditions have been simulated under constant flow rate boundary condition at different wettability conditions. Our results shows that the relation between the half corner angle of pores and contact angle controls the temporal evolution of capillary pressure during the invasion of a pore. By deviating from pure water-wet conditions, a dip in the temporal evolution of capillary pressure can be observed which will be pronounced in irregular angular cross sections. That enhances the pore invasion with a smaller differential pressure. The interplay between the contact angle and pore geometry can have significant implications for enhanced remobilization of ganglia in intermediate contact angles in real porous media morphologies, where pores are very heterogeneous with small shape factors. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

  6. Trapping of hydride forming elements within miniature electrothermal devices. Part 2. Investigation of collection of arsenic and selenium hydrides on a surface and in a cavity of a graphite rod

    International Nuclear Information System (INIS)

    Docekal, Bohumil

    2004-01-01

    The interaction of arsenic and selenium hydrides with bare and modified graphite was investigated by atomic absorption spectrometry and by radiotracer technique using 75 Se radionuclide in a laboratory made brass cylindrical chamber equipped with a vertical quartz tube torch for supporting miniature hydrogen diffusion flame atomizer. Strong interaction was observed at elevated temperatures above 800 deg. C. In contrast to the very often-reported data for conventional graphite tube atomizers, this high temperature interaction was also accompanied by a pronounced trapping of analytes at elevated temperatures close to 1100-1200 deg. C when modified graphite was used. Comparing modifiers tested (Ir, Pt and Rh), iridium appeared the only useful permanent modifier. Among various graphite-rod traps designed, the most efficient trapping of analytes was achieved in a graphite cavity. The net selenium trapping efficiencies of approximately 53% and 70% were found by radiotracer technique for the iridium-treated graphite surface and the iridium-treated graphite cavity, respectively. In contrast to the molybdenum surface, bare graphite did not exhibit any significant trapping effect. Trapping isotherms obtained at different temperatures displayed non-linear course in the range up to the upper limit of the analytical relevance of 100 ng of an analyte, indicating a limited trapping capacity of the modified graphite surface and the same trapping mechanism at low and elevated temperatures applied (300-1300 deg. C). Radiography experiments with 75 Se radiotracer showed that a major part of selenium was collected within the small cavity of the graphite rod and that selenium was also deposited after the trapping and vaporization steps in the trap chamber and on the quartz tube wall of the burner. Complementary experiments performed with the conventional transversally heated graphite tube and with bare and thermally shielded injection capillaries for hydride introduction, showed that

  7. The Moderating Role of Purging Behaviour in the Relationship Between Sexual/Physical Abuse and Nonsuicidal Self-Injury in Eating Disorder Patients.

    Science.gov (United States)

    Gonçalves, Sónia; Machado, Bárbara; Silva, Cátia; Crosby, Ross D; Lavender, Jason M; Cao, Li; Machado, Paulo P P

    2016-03-01

    This study sought to examine predictors of nonsuicidal self-injury (NSSI) in eating disorder patients and to evaluate the moderating role of purging behaviours in the relationship between a theorised predictor (i.e. sexual/physical abuse) and NSSI. Participants in this study were 177 female patients with eating disorders (age range = 14-38 years) who completed semistructured interviews assessing eating disorder symptoms and eating disorder-related risk factors (e.g. history of sexual and physical abuse, history of NSSI and feelings of fatness). Results revealed that 65 participants (36.7%) reported lifetime engagement in NSSI, and 48 participants (27.1%) reported a history of sexual/physical abuse. Early onset of eating problems, lower BMI, feeling fat, a history of sexual/physical abuse and the presence of purging behaviours were all positively associated with the lifetime occurrence of NSSI. The relationship between sexual/physical abuse before eating disorder onset and lifetime NSSI was moderated by the presence of purging behaviours, such that the relationship was stronger in the absence of purging. These findings are consistent with the notion that purging and NSSI may serve similar functions in eating disorder patients (e.g. emotion regulation), such that the presence of purging may attenuate the strength of the association between sexual/physical abuse history (which is also associated with elevated NSSI risk) and engagement in NSSI behaviours. Copyright © 2015 John Wiley & Sons, Ltd and Eating Disorders Association.

  8. Isotopic fractionation of fentanyl and its deuterated analogues by capillary gas chromatography

    International Nuclear Information System (INIS)

    Sera, Shoji; Goromaru, Tsuyoshi

    1997-01-01

    Isotopic fractionation of fentanyl (FT) and its deuterated analogues by gas chromatography using capillary columns (CBP1 and CBP5) has been investigated. Seven kinds of analogues were labeled with 5 to 19 deuterium atoms at the anilino, propionyl and/or phenylethyl group of FT. The retention times of deuterated FT in CBP1 and CBP5 columns are inversely proportional to the number of labeled deuterium atoms in the molecule. The difference in free enegy changes (ΔΔG) had a linear relationship with the number of labeled deuterium atoms, except for labeling at anilino and phenylethyl group. The contribution of a deuterium atom to the ΔΔG value was estimated to be 1.13 cal/mol in CBP1 and 1.40 cal/mol in CBP5, respectively. While, its contribution in the propiony group was 2.84 cal/mol in CBP1 and 2.48 cal/mol in CBP5, respectively. An important factor in separation by GC may differences in interactions between the stationary phase of the column with the three dimensional protrusive moiety in the molecule. (author)

  9. Isotopic fractionation of fentanyl and its deuterated analogues by capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan)

    1997-12-01

    Isotopic fractionation of fentanyl (FT) and its deuterated analogues by gas chromatography using capillary columns (CBP1 and CBP5) has been investigated. Seven kinds of analogues were labeled with 5 to 19 deuterium atoms at the anilino, propionyl and/or phenylethyl group of FT. The retention times of deuterated FT in CBP1 and CBP5 columns are inversely proportional to the number of labeled deuterium atoms in the molecule. The difference in free enegy changes ({Delta}{Delta}G) had a linear relationship with the number of labeled deuterium atoms, except for labeling at anilino and phenylethyl group. The contribution of a deuterium atom to the {Delta}{Delta}G value was estimated to be 1.13 cal/mol in CBP1 and 1.40 cal/mol in CBP5, respectively. While, its contribution in the propiony group was 2.84 cal/mol in CBP1 and 2.48 cal/mol in CBP5, respectively. An important factor in separation by GC may differences in interactions between the stationary phase of the column with the three dimensional protrusive moiety in the molecule. (author)

  10. Hysteretic growth and decay of a waterspout column

    Science.gov (United States)

    Naumov, Igor V.; Herrada, Miguel A.; Sharifullin, Bulat R.; Shtern, Vladimir N.

    2018-02-01

    This work explores a model waterspout: a flow of water and sunflower oil driven by the rotating lid in a sealed vertical cylindrical container. The experiments reveal the hysteretic growth and decay of a water column. The numerical simulations uncover vortex breakdown (VB) in the water and oil flows. As the rotation speeds up, (1) a VB water cell emerges near the bottom center, (2) it expands and occupies almost the entire water volume except a thin layer adjusted to the interface, (3) a VB oil cell emerges and disappears above the interface-axis intersection, (4) the interface rises near the axis, descends at the periphery, and shifts from the sidewall to the bottom, (5) the water touches the lid near the axis and forms a column, extending from the bottom up to the lid. As the rotation decelerates, the process reverses, but the flow states differ from those for the direct process at same rotation speeds. It is argued that the hysteresis is a capillary phenomenon and occurs because the interface-wall contact angle differs in the direct and reverse processes.

  11. Autologous bone marrow purging with LAK cells.

    Science.gov (United States)

    Giuliodori, L; Moretti, L; Stramigioli, S; Luchetti, F; Annibali, G M; Baldi, A

    1993-12-01

    In this study we will demonstrate that LAK cells, in vitro, can lyse hematologic neoplastic cells with a minor toxicity of the staminal autologous marrow cells. In fact, after bone marrow and LAK co-culture at a ratio of 1/1 for 8 hours, the inhibition on the GEMM colonies resulted to be 20% less compared to the untreated marrow. These data made LAK an inviting agent for marrow purging in autologous bone marrow transplantation.

  12. Dynamic performance of a high-temperature PEM (proton exchange membrane) fuel cell – Modelling and fuzzy control of purging process

    International Nuclear Information System (INIS)

    Zhang, Caizhi; Liu, Zhitao; Zhang, Xiongwen; Chan, Siew Hwa; Wang, Youyi

    2016-01-01

    To improve fuel utilization of HT-PEMFC (high-temperature proton exchange membrane fuel cell), which normally operates under dead-end mode, with properly periodical purging to flush out the accumulated water vapour in the anode flow-field is necessary, otherwise the performance of HT-PEMFC would drop gradually. In this paper, a semi-empirical dynamic voltage model of HT-PEMFC is developed for controller design purpose via fitting the experimental data and validated with experimental results. Then, a fuzzy controller is designed to schedule the purging based on the obtained model. According to the result, the developed model well reflects transient characteristics of HT-PEMFC voltage and the fuzzy controller offers good performance for purging scheduling under uncertain load demands. - Highlights: • A semi-empirical dynamic voltage model of HT-PEMFC is developed for control design. • The model is developed via fitting and validated with experimental results. • A fuzzy controller is designed to schedule the purging based on the obtained model.

  13. Evaluation of Carbon Nanotubes Functionalized Polydimethylsiloxane Based Coatings for In-Tube Solid Phase Microextraction Coupled to Capillary Liquid Chromatography

    OpenAIRE

    Neus Jornet-Martínez; Pascual Serra-Mora; Yolanda Moliner-Martínez; Rosa Herráez-Hernández; Pilar Campíns-Falcó

    2015-01-01

    In the present work, the performance of carbon nanotubes (c-CNTs) functionalized polydimethylsiloxane (PDMS) based coatings as extractive phases for in-tube solid phase microextraction (IT-SPME) coupled to Capillary LC (CapLC) has been evaluated. Carboxylic-single walled carbon nanotubes (c-SWNTs) and carboxylic-multi walled carbon nanotubes (c-MWNTs) have been immobilized on the activated surface of PDMS capillary columns. The effect of different percentages of diphenyl groups in the PDMS ex...

  14. Research Article. The Influence of Some Parameters on Chiral Separation of Ibuprofen by High-Performance Liquid Chromatography and Capillary Electrophoresis

    Directory of Open Access Journals (Sweden)

    Balint Alina

    2017-03-01

    Full Text Available Objective: The aim of the study was to compare the influence of mobile phase composition and temperature on chiral separation of racemic ibuprofen by capillary electrophoresis and high performance liquid chromatography with UV detection. Materials and methods: Racemic ibuprofen was analysed on a chiral OVM column with an HPLC system 1100 Agilent Technologies, under isocratic elution, by using potassium dihydrogen phosphate 20 mM and ethanol in mobile phase. The flow rate was set at 1 mL/min, UV detector at 220 nm and different column temperatures were tested. For electrophoresis separation an Agilent CE G1600AX Capillary Electrophoresis System system, with UV detection, was used. The electrophoresis analysis was performed at different pH values and temperatures, with phosphate buffer 25 mM and methyl-β-cyclodextrin as chiral selector. Results: The chromatograhic analysis reveals a high influence of mobile phase pH on ibuprofen enantiomers separation. An elution with a mixture of potassium dihydrogen phosphate 20 mM pH=3 and ethanol, at 25°C, allowed enantiomers separation with good resolution in less than 8 min. Conclusions: The proposed HPLC method proved suitable for the separation of ibuprofen enantiomers with a good resolution, but the capillary electrophoresis tested parameters did not allow chiral discrimination.

  15. FMECA about pre-treatment system for purge gas of test blanket module in ITER

    International Nuclear Information System (INIS)

    Fu Wanfa; Luo Deli; Tang Tao

    2012-01-01

    The pre-treatment system for purge gas of TBM will be installed in Port Cell for installing TBM in ITER, the function of which includes filtering purge gas, removing HTO, cooling, and adjusting flow rate, etc. The purge gas treated will be conveyed into TES (Tritium Extraction System). The technological process and system components in pre-treatment system were introduced. Tritium releasing risk was regarded as failure criterion; failure mode, effects and criticality analysis (FMECA) were carried out and several weaknesses or failure mode in the system were found. Besides, risk priority number (RPN) and failure mode criticality were calculated. Finally, some design improvement measures and usage compensation measures were given. At last, four important potential failure modes were found out. The analysis will provide the design basis for reducing risk of excessive tritium releasing, which is also a useful assist for safety analysis about other tritium system. (authors)

  16. Initial post dynamic buckling of a quadratic-cubic column ...

    African Journals Online (AJOL)

    In this investigation, we determine the dynamic buckling load of an imperfect finite column resting on a mixed quadratic-cubic nonlinear elastic foundation trapped by an explicitly time dependent sinusoidally slowly varying dynamic load .The resultant coefficients are dynamically slowly varying and the formulation contains ...

  17. Application of capillary electrophoresis to anion speciation in soil water extracts: 2. Arsenic

    Energy Technology Data Exchange (ETDEWEB)

    Naidu, R.; Smith, J.; McLaren, R.G.; Stevens, D.P.; Sumner, M.E.; Jackson, P.E.

    2000-02-01

    A method has been developed for the speciation of arsenic (AsO{sub 2}{sup {minus}}, AsO{sub 4}{sup 3{minus}}, and dimethylarsinic [DMA]) in natural soil solutions from contaminated sites in Australia. The separation of these anions was achieved by capillary zone electrophoresis (CZE) using a fused silica capillary with a basic chromate buffer and on-column indirect UV detection at 254 nm. Method parameters, such as electrolyte pH, run voltage, and capillary temperature were studied in order to establish suitable analytical conditions. The ideal separation for As(III) and DMA was achieved with a buffer pH of 8.0, a run voltage of 25 kV, and a capillary temperature of 30 C. Under these conditions, As(V) and orthophosphate ions comigrated. However, the use of a chromate buffer at pH 10, a run voltage of 20 kV, and capillary temperature of 20 C led to complete separation of As(V) and phosphate peaks. Results of these investigations together with recovery test data suggest that separation of the As species from soil solutions can be achieved in less than 5 min with detection limits of 0.50, 0.10, and 0.10 mg L{sup {minus}1} for As(III), As(V), and DMA, respectively.

  18. Physical Sequestration of Bacillus anthracis in the Pulmonary Capillaries in Terminal Infection.

    Science.gov (United States)

    Jouvion, Gregory; Corre, Jean-Philippe; Khun, Huot; Moya-Nilges, Marie; Roux, Pascal; Latroche, Claire; Tournier, Jean-Nicolas; Huerre, Michel; Chrétien, Fabrice; Goossens, Pierre L

    2016-07-15

    The lung is the terminal target of Bacillus anthracis before death, whatever the route of infection (cutaneous, inhalational, or digestive). During a cutaneous infection in absence of toxins, we observed encapsulated bacteria colonizing the alveolar capillary network, bacteria and hemorrhages in alveolar and bronchiolar spaces, and hypoxic foci in the lung (endothelial cells) and brain (neurons and neuropil). Circulating encapsulated bacteria were as chains of approximately 13 µm in length. Bacteria of such size were immediately trapped within the lung capillary network, but bacteria of shorter length were not. Controlling lung-targeted pathology would be beneficial for anthrax treatment. © The Author 2016. Published by Oxford University Press for the Infectious Diseases Society of America. All rights reserved. For permissions, e-mail journals.permissions@oup.com.

  19. Photodeposited silver nanoparticles for on-column surface-enhanced Raman spectrometry detection in capillary electrophoresis

    Czech Academy of Sciences Publication Activity Database

    Přikryl, Jan; Klepárník, Karel; Foret, František

    2012-01-01

    Roč. 1226, - (2012), s. 43-47 ISSN 0021-9673 R&D Projects: GA ČR GA203/08/1680; GA ČR(CZ) GAP301/11/2055; GA MŠk LC06023 Institutional research plan: CEZ:AV0Z40310501 Keywords : SERS * capillary electrophoresis * photodeposition Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.612, year: 2012

  20. Confocal laser-induced fluorescence detector for narrow capillary system with yoctomole limit of detection.

    Science.gov (United States)

    Weaver, Mitchell T; Lynch, Kyle B; Zhu, Zaifang; Chen, Huang; Lu, Joann J; Pu, Qiaosheng; Liu, Shaorong

    2017-04-01

    Laser-induced fluorescence (LIF) detectors for low-micrometer and sub-micrometer capillary on-column detection are not commercially available. In this paper, we describe in details how to construct a confocal LIF detector to address this issue. We characterize the detector by determining its limit of detection (LOD), linear dynamic range (LDR) and background signal drift; a very low LOD (~70 fluorescein molecules or 12 yoctomole fluorescein), a wide LDR (greater than 3 orders of magnitude) and a small background signal drift (~1.2-fold of the root mean square noise) are obtained. For detecting analytes inside a low-micrometer and sub-micrometer capillary, proper alignment is essential. We present a simple protocol to align the capillary with the optical system and use the position-lock capability of a translation stage to fix the capillary in position during the experiment. To demonstrate the feasibility of using this detector for narrow capillary systems, we build a 2-μm-i.d. capillary flow injection analysis (FIA) system using the newly developed LIF prototype as a detector and obtain an FIA LOD of 14 zeptomole fluorescein. We also separate a DNA ladder sample by bare narrow capillary - hydrodynamic chromatography and use the LIF prototype to monitor the resolved DNA fragments. We obtain not only well-resolved peaks but also the quantitative information of all DNA fragments. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Development of high power pumping system for capillary discharge EUV laser

    International Nuclear Information System (INIS)

    Sakai, Yusuke; Komatsu, Takanori; Watanabe, Masato; Okino, Akitoshi; Hotta, Eiki

    2008-01-01

    Development of high power pumping system for capillary discharge soft X-ray laser is reported. The pulsed power system consists of a 2.2 μF LC generator, a 2:54 step-up transformer and a 3 nF water capacitor. Taking advantage of high efficiency configuration, step-up ratio of water capacitor voltage to LC generator initial voltage is about 40 times. Consequently, obtained water capacitor voltage reaches about 450 kV when LC generator was charged to 12.5 kV. As a consequent, possibility of charging a water capacitor to 1 MV is demonstrated. With this extremely compact system, discharge current could be increased to nearly 100 kA through moderately long capillary, which leads to generation of high-density and high-temperature plasma column in order to realize EUV laser. (author)

  2. Single-step reinforced microextraction of polycyclic aromatic hydrocarbons from soil samples using an inside needle capillary adsorption trap with electropolymerized aniline/multi-walled carbon nanotube sorbent.

    Science.gov (United States)

    Ghiasvand, Ali Reza; Yazdankhah, Fatemeh

    2017-03-03

    A polyaniline/multi-wall carbon nanotubes (PANI/MWCNT) composite was electrodeposited on the interior surface of a platinized stainless steel capillary needle and used to prepare an inside needle capillary adsorption trap (INCAT) device. The platinization expanded the interior adsorbing surface of the needle and made it more porous and cohesive for nanocomposite film. The nanocomposite was characterized using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). The fabricated INCAT was fixed into a cooling capsule to fabricate a cooling-assisted INCAT (CA-INCAT) system. The CA-INCAT device was used to extract polycyclic aromatic hydrocarbons (PAHs) from solid samples followed by gas chromatography-flame ionization detection (GC-FID) determination. To obtain the best extraction efficiency, the important experimental variables were studied and optimized. Under the optimal conditions, the limits of detection (LODs) for the studied PAHs were in the range of 0.002-0.02ngg -1 . Linear dynamic ranges (LDRs) for the calibration curves were found to be 0.1-30,000ngg -1 . Relative standard deviations (RSDs%) for six replicated analysis of 1ngg -1 PAHs were obtained 7.7-11%. The CA-INCAT-GC-FID method was successfully applied for the extraction and determination of PAHs in contaminated soil samples. The results were in agreement with those obtained by a validated ultrasound-assisted solvent extraction (UA-SE) method. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Capillary electrophoresis of chitooligosaccharides in acidic solution: simple determination using a quaternary-ammonium-modified column and indirect photometric detection with crystal violet.

    Science.gov (United States)

    Hattori, Toshiaki; Anraku, Nobuhiro; Kato, Ryo

    2010-02-01

    Five chitosan oligosaccharides were separated in acidic aqueous solution by capillary electrophoresis (CE) with indirect photometric detection using a positively coated capillary. Electrophoretic mobility of the chitooligosaccharides (COSs) depended on the number of monomer units in acidic aqueous solution, similar to other polyelectrolyte oligomers. The separation was developed in nitric acid aqueous solution at pH 3.0 with 1 mM Crystal Violet, using a capillary positively coated with N-trimethoxypropyl-N,N,N-trimethylammonium chloride. The limit of the detection for chitooligosaccharides with two to six saccharide chains was less than 5 microM. CE determination of an enzymatically hydrolyzed COS agreed with results from HPLC. 2009 Elsevier B.V. All rights reserved.

  4. Water movement in glass bead porous media: 1. Experiments of capillary rise and hysteresis

    Science.gov (United States)

    Lu, T. X.; Biggar, J. W.; Nielsen, D. R.

    1994-12-01

    Experimental observations of capillary rise and hysteresis of water or ethanol in glass beads are presented to improve our understanding of those physical processes in porous media. The results provide evidence that capillary rise into porous media cannot be fully explained by a model of cylinders. They further demonstrate that the "Ink bottle" model does not provide an adequate explanation of hysteresis. Glass beads serving as a model for ideal soil are enclosed in a rectangular glass chamber model. A TV camera associated with a microscope was used to record the processes of capillary rise and drainage. It is clearly shown during capillary rise that the fluid exhibits a "jump" behavior at the neck of the pores in an initially dry profile or at the bottom of the water film in an initially wet profile. Under an initially dry condition, the jump initiates at the particle with smallest diameter. The jump process continues to higher elevations until at equilibrium the surface tensile force is balanced by the hydrostatic force. The wetting front at that time is readily observed as flat and saturated. Under an initially wet condition, capillary rise occurs as a water film thickening process associated with the jump process. Trapped air behind the wetting front renders the wetting front irregular and unsaturated. The capillary rise into an initially wet porous medium can be higher than that into an initially dry profile. During the drying process, large surface areas associated with the gas-liquid interface develop, allowing the porous medium to retain more water than during the wetting process at the same pressure. That mechanism explains better the hysteresis phenomenon in porous media in contrast to other mechanisms that now prevail.

  5. Spent Nuclear Fuel (SNF) Project Cask and MCO Helium Purge System Design Review Completion Report - Project A.5 and A.6

    International Nuclear Information System (INIS)

    ARD, K.E.

    2000-01-01

    This report documents the results of the design verification performed on the Cask and Multiple Canister Over-pack (MCO) Helium Purge System. The helium purge system is part of the Spent Nuclear Fuel (SNF) Project Cask Loadout System (CLS) at 100K area. The design verification employed the ''Independent Review Method'' in accordance with Administrative Procedure (AP) EN-6-027-01

  6. Effect of air on water capillary flow in silica nanochannels

    DEFF Research Database (Denmark)

    Zambrano, Harvey; Walther, Jens Honore; Oyarzua, Elton

    2013-01-01

    , with the fabrication of microsystems integrated by nanochannels, a thorough understanding of the transport of fluids in nanoconfinement is required for a successful operation of the functional parts of such devices. In this work, Molecular Dynamics simulations are conducted to study the spontaneous imbibition of water...... in sub 10 nm silica channels. The capillary filling speed is computed in channels subjected to different air pressures. In order to describe the interactions between the species, an effective force field is developed, which is calibrated by reproducing the water contact angle. The results show...... that the capillary filling speed qualitatively follows the classical Washburn model, however, quantitatively it is lower than expected. Furthermore, it is observed that the deviations increase as air pressure is higher. We attribute the deviations to amounts of air trapped at the silica-water interface which leads...

  7. The analysis of semi-volatile and non-volatile petroleum hydrocarbons in a soil/sediment matrix by capillary column gas chromatography/flame ionization detection (GC/FID)

    International Nuclear Information System (INIS)

    George, J.E. III; Thoma, J.J.; Hastings, M.

    1990-01-01

    A comprehensive analysis for semi-volatile and non-volatile fractions of petroleum hydrocarbons can be achieved by a solvent extraction/concentration techniques that will effectively extract these high molecular weight fractions from a soil matrix. The prepared extract is then injected directly into a gas chromatograph equipped with a capillary column and flame ionization detector. This technique applies to the following types of commercially available petroleum hydrocarbons: Diesel Nos. 2,4,5, and 6, fuel oils and several grades of lubrication oil. The identification of a particular petroleum hydrocarbon is determined visually by comparison of the samples with known hydrocarbon standards. Accurate quantitation of the chromatograms is possible by using peak area summation and the presence of an internal standard. The practical quantitation limit for the method is 10 mg/Kg for most fuel types. This paper presents a method for determining the concentration of these fuel types in soil. Data will be presented only on 10W40 lubrication oil in terms of method validation, calibration, percent recovery, and method detection limits. A discussion of the quatitation techniques used will also be included

  8. Incorporation of metal-organic framework HKUST-1 into porous polymer monolithic capillary columns to enhance the chromatographic separation of small molecules.

    Science.gov (United States)

    Yang, Shengchao; Ye, Fanggui; Lv, Qinghui; Zhang, Cong; Shen, Shufen; Zhao, Shulin

    2014-09-19

    Metal-organic framework (MOF) HKUST-1 nanoparticles have been incorporated into poly(glycidyl methacrylate-co-ethylene dimethacrylate) (HKUST-1-poly(GMA-co-EDMA)) monoliths to afford stationary phases with enhanced chromatographic performance of small molecules in the reversed phase capillary liquid chromatography. The effect of HKUST-1 nanoparticles in the polymerization mixture on the performance of the monolithic column was explored in detail. While the bare poly(GMA-co-EDMA) monolith exhibited poor resolution (RsHKUST-1 nanoparticles to the polymerization mixture provide high increased resolution (Rs≥1.3) and high efficiency ranged from 16,300 to 44,300plates/m. Chromatographic performance of HKUST-1-poly(GMA-co-EDMA) monolith was demonstrated by separation of various analytes including polycyclic aromatic hydrocarbons, ethylbenzene and styrene, phenols and aromatic acids using a binary polar mobile phase (CH3CN/H2O). The HKUST-1-poly(GMA-co-EDMA) monolith displayed enhanced hydrophobic and π-π interaction characteristics in the reversed phase separation of test analytes compared to the bare poly(GMA-co-EDMA) monolith. The experiment results showed that HKUST-1-poly(GMA-co-EDMA) monoliths are an alternative to enhance the chromatographic separation of small molecules. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Direct measurement of the wetting front capillary pressure in a clay brick ceramic

    Energy Technology Data Exchange (ETDEWEB)

    Ioannou, Ioannis [Manchester Centre for Civil and Construction Engineering, UMIST, PO Box 88, Manchester M60 1QD (United Kingdom); Hall, Christopher [Centre for Materials Science and Engineering and School of Engineering and Electronics, University of Edinburgh, The King' s Buildings, Edinburgh EH9 3JL (United Kingdom); Wilson, Moira A [Manchester Centre for Civil and Construction Engineering, UMIST, PO Box 88, Manchester M60 1QD (United Kingdom); Hoff, William D [Manchester Centre for Civil and Construction Engineering, UMIST, PO Box 88, Manchester M60 1QD (United Kingdom); Carter, Margaret A [Manchester Centre for Civil and Construction Engineering, UMIST, PO Box 88, Manchester M60 1QD (United Kingdom)

    2003-12-21

    The absorption of a liquid into a rectangular bar of an initially dry porous material that is sealed on all surfaces except the inflow face is analysed in terms of Sharp Front theory. Sharp Front models are developed for both complete and incomplete displacement of air ahead of the advancing wetting front. Experiments are described from which a characteristic capillary potential of the material is obtained by measuring the equilibrium pressure of the air displaced and compressed ahead of the advancing wetting front. Results for the absorption of water and n-heptane by a fired clay brick ceramic suggest that this wetting front capillary pressure (or capillary potential) scales approximately with the surface tension and also that the permeability scales inversely with the liquid viscosity. The pressure of the air trapped in the wetted region is found to be the same as the pressure of the displaced air. For this material the wetting front capillary pressure for water at 20 C is 0.113 MPa, equivalent to a hydraulic tension head of 11.5 m and to a Young-Laplace pore diameter of 2.6 {mu}m. The capillary pressure so measured is apparently a fundamental percolation property of the material that can be interpreted as the air pressure at which liquid phase continuity and unsaturated conductivity both vanish. The method described can be applied generally to porous materials.

  10. Direct measurement of the wetting front capillary pressure in a clay brick ceramic

    International Nuclear Information System (INIS)

    Ioannou, Ioannis; Hall, Christopher; Wilson, Moira A; Hoff, William D; Carter, Margaret A

    2003-01-01

    The absorption of a liquid into a rectangular bar of an initially dry porous material that is sealed on all surfaces except the inflow face is analysed in terms of Sharp Front theory. Sharp Front models are developed for both complete and incomplete displacement of air ahead of the advancing wetting front. Experiments are described from which a characteristic capillary potential of the material is obtained by measuring the equilibrium pressure of the air displaced and compressed ahead of the advancing wetting front. Results for the absorption of water and n-heptane by a fired clay brick ceramic suggest that this wetting front capillary pressure (or capillary potential) scales approximately with the surface tension and also that the permeability scales inversely with the liquid viscosity. The pressure of the air trapped in the wetted region is found to be the same as the pressure of the displaced air. For this material the wetting front capillary pressure for water at 20 C is 0.113 MPa, equivalent to a hydraulic tension head of 11.5 m and to a Young-Laplace pore diameter of 2.6 μm. The capillary pressure so measured is apparently a fundamental percolation property of the material that can be interpreted as the air pressure at which liquid phase continuity and unsaturated conductivity both vanish. The method described can be applied generally to porous materials

  11. Impacts on oil recovery from capillary pressure and capillary heterogeneities

    Energy Technology Data Exchange (ETDEWEB)

    Bognoe, Thomas

    2008-07-01

    The main conclusions drawn from this thesis are; 7 scientific papers are published on a broad variety of subjects, and describes in detail the experiments and research treated in this thesis. Scientific research has been performed, investigating the subjects of capillary pressure and capillary heterogeneities from different angles. This thesis discusses the findings in this study and aims to illustrate the benefits of the results obtained for further development of other experiments, and/or even the industrial benefits in field development. The methods for wettability alteration have developed throughout the work. From producing heterogeneous wettability alterations, the methods have improved to giving both radial and lateral uniform wettability alterations, which also remains unaltered throughout the duration of the experimental work. The alteration of wettability is dependent on initial water saturation, flow rate, aging time and crude oil composition. Capillary pressure and relative permeability curves have been measured for core plugs at different wettabilities using conventional centrifuge methods. The trends observed are mostly consistent with theory. The production mechanisms of strongly and moderately water wet chalk has been investigated. At strongly water wet conditions in fractured chalk; the flow is governed by capillary forces, showing strong impact from the fractures. At moderately water wet conditions, the impact of the fractures are absent, and a dispersed water front is observed during the displacement. The oil recovery is about the same, at the two wettabilities. Fracture crossing mechanisms at the same wettability conditions have been mapped. And the observations are consistent with those of the water floods. During strongly water wet displacement, the fracture crossing is occurring once the inlet core has reached endpoint of spontaneous imbibition. At moderately water wet conditions the fracture crossing is less abrupt, and creation of wetting

  12. Periodic imidazolium-bridged hybrid monolith for high-efficiency capillary liquid chromatography with enhanced selectivity.

    Science.gov (United States)

    Qiao, Xiaoqiang; Zhang, Niu; Han, Manman; Li, Xueyun; Qin, Xinying; Shen, Shigang

    2017-03-01

    A novel periodic imidazolium-bridged hybrid monolithic column was developed. With diene imidazolium ionic liquid 1-allyl-3-vinylimidazolium bromide as both cross-linker and organic functionalized reagent, a new periodic imidazolium-bridged hybrid monolithic column was facilely prepared in capillary with homogeneously distributed cationic imidazolium by a one-step free-radical polymerization with polyhedral oligomeric silsesquioxane methacryl substituted. The successful preparation of the new column was verified by Fourier transform infrared spectroscopy, scanning electron microscopy, elemental analysis, and surface area analysis. Most interestingly, the bonded amount of 1-allyl-3-vinylimidazolium bromide of the new column is three times higher than that of the conventional imidazolium-embedded hybrid monolithic column and the specific surface area of the column reached 478 m 2 /g. The new column exhibited high stability, excellent separation efficiency, and enhanced separation selectivity. The column efficiency reached 151 000 plates/m for alkylbenzenes. Furthermore, the new column was successfully used for separation of highly polar nucleosides and nucleic acid bases with pure water as mobile phase and even bovine serum albumin tryptic digest. All these results demonstrate the periodic imidazolium-bridged hybrid monolithic column is a good separation media and can be used for chromatographic separation of small molecules and complex biological samples with high efficiency. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

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

    2014-11-28

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

  14. Bulimia Nervosa/Purging Disorder.

    Science.gov (United States)

    Castillo, Marigold; Weiselberg, Eric

    2017-04-01

    Bulimia nervosa was first described in 1979 by British psychiatrist Gerald Russell as a "chronic phase of anorexia nervosa" in which patients overeat and then use compensatory mechanisms, such as self-induced vomiting, laxatives, or prolonged periods of starvation. The characterization of bulimia nervosa continues to evolve with the introduction of the DSM-5 in 2013. In this article, the epidemiology and risk factors of bulimia nervosa are identified and reviewed, along with the medical complications and psychiatric comorbidities. The evaluation of a patient with suspected bulimia nervosa is addressed, with an emphasis on acquiring a complete and thorough history as well as discovering any comorbidities that are present. Management of the patient involves both medical interventions and behavioral counseling in order to address physical, psychological, and social needs. Lastly, a new diagnosis introduced in the DSM-5, purging disorder, is described and discussed. Copyright © 2017 Mosby, Inc. All rights reserved.

  15. Determination of Betaine in Forsythia Suspensa by High Performance Capillary Electrophoresis

    Science.gov (United States)

    Liu, Haixing; Dong, Guoliang; Wang, Lintong

    2017-12-01

    This paper presents the determination of betaine content of Forsythia suspensa by high performance capillary electrophoresis (HPCE) method. The borax solution was chosen as buffer solution, and its concentration was 40 mmol with capillary column (75μm×52/60cm) at a constant voltage of 20kV and injecting pressure time of 10s at 20°C. Linearity was kept in the concent ration range of 0.0113-1.45mg·ml-1 of betaine with correlation coefficient of 0.999. The recovery was in the range of 97%-117% (n=5), The content of betaine was 281.5 mg·g-1and RSD value of 9.6% (n=6) in Forsythia suspensa. This method has the advantage of rapid, accurate and good repeatability in separation and determination of betaine in Forsythia suspensa.

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

    Science.gov (United States)

    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.

  17. An implantable centrifugal blood pump with a recirculating purge system (Cool-Seal system).

    Science.gov (United States)

    Yamazaki, K; Litwak, P; Tagusari, O; Mori, T; Kono, K; Kameneva, M; Watach, M; Gordon, L; Miyagishima, M; Tomioka, J; Umezu, M; Outa, E; Antaki, J F; Kormos, R L; Koyanagi, H; Griffith, B P

    1998-06-01

    A compact centrifugal blood pump has been developed as an implantable left ventricular assist system. The impeller diameter is 40 mm, and pump dimensions are 55 x 64 mm. This first prototype, fabricated from titanium alloy, resulted in a pump weight of 400 g including a brushless DC motor. The weight of a second prototype pump was reduced to 280 g. The entire blood contacting surface is coated with diamond like carbon (DLC) to improve blood compatibility. Flow rates of over 7 L/min against 100 mm Hg pressure at 2,500 rpm with 9 W total power consumption have been measured. A newly designed mechanical seal with a recirculating purge system (Cool-Seal) is used for the shaft seal. In this seal system, the seal temperature is kept under 40 degrees C to prevent heat denaturation of blood proteins. Purge fluid also cools the pump motor coil and journal bearing. Purge fluid is continuously purified and sterilized by an ultrafiltration unit which is incorporated in the paracorporeal drive console. In vitro experiments with bovine blood demonstrated an acceptably low hemolysis rate (normalized index of hemolysis = 0.005 +/- 0.002 g/100 L). In vivo experiments are currently ongoing using calves. Via left thoracotomy, left ventricular (LV) apex descending aorta bypass was performed utilizing an expanded polytetrafluoroethylene (ePTFE) vascular graft with the pump placed in the left thoracic cavity. In 2 in vivo experiments, the pump flow rate was maintained at 5-9 L/min, and pump power consumption remained stable at 9-10 W. All plasma free Hb levels were measured at less than 15 mg/dl. The seal system has demonstrated good seal capability with negligible purge fluid consumption (<0.5 ml/day). In both calves, the pumps demonstrated trouble free continuous function over 6 month (200 days and 222 days).

  18. Preliminary assessment of laboratory techniques for measurement of volatiles through soils at hazardous waste sites

    International Nuclear Information System (INIS)

    Breckenridge, R.P.; Case, J.T.

    1985-01-01

    This study was conducted to determine if an inexpensive laboratory screening technique could be developed to detect the presence of hazardous volatile compounds without disturbing the soil over buried waste. A laboratory investigation was designed to evaluate the movement of two volatile organics through packed soil columns. Six soil columns were filled with three different soils. Two volatile organics, trichloroethylene (TCE) and dichloroethylene (1, 2 DCE), were placed at the base of the columns as a saturated water solution. Column headspace analysis was performed by purging the top of the columns with nitrogen gas and bubbling this gas through a pentane trap. Samples in the air space were also collected using 25 and 100 microliter gas tight syringes. All samples were analyzed using Electron Capture Detector (ECD) by gas chromatography. Results indicate that the volatile organic compounds can be detected through a five foot column of soil in concentrations down to parts-per-billion (ppb) for both TCE and DCE. Distribution coefficients (Kd) experiments were also conducted to assess breakthrough time and related concentration with soil type

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

    Science.gov (United States)

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

    2015-01-02

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

  20. Sub-mm Scale Fiber Guided Deep/Vacuum Ultra-Violet Optical Source for Trapped Mercury Ion Clocks

    Science.gov (United States)

    Yi, Lin; Burt, Eric A.; Huang, Shouhua; Tjoelker, Robert L.

    2013-01-01

    We demonstrate the functionality of a mercury capillary lamp with a diameter in the sub-mm range and deep ultraviolet (DUV)/ vacuum ultraviolet (VUV) radiation delivery via an optical fiber integrated with the capillary. DUV spectrum control is observed by varying the fabrication parameters such as buffer gas type and pressure, capillary diameter, electrical resonator design, and temperature. We also show spectroscopic data of the 199Hg+ hyper-fine transition at 40.5GHz when applying the above fiber optical design. We present efforts toward micro-plasma generation in hollow-core photonic crystal fiber with related optical design and theoretical estimations. This new approach towards a more practical DUV optical interface could benefit trapped ion clock developments for future ultra-stable frequency reference and time-keeping applications.

  1. Topographical properties of polymer films deposited in capillaries for electrophoretic separations of large organic molecules

    Czech Academy of Sciences Publication Activity Database

    Guryča, Vilém; Pacáková, V.; Tlusťáková, Marie; Štulík, K.; Michálek, Jiří

    2004-01-01

    Roč. 27, č. 13 (2004), s. 1121-1129 ISSN 1615-9306 R&D Projects: GA AV ČR IBS4050005; GA AV ČR KSK4055109 Institutional research plan: CEZ:AV0Z4050913 Keywords : capillary electrophoresis * hydrogel polymer coating * column technology Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.927, year: 2004

  2. Seasonal patterns of birth for subjects with bulimia nervosa, binge eating, and purging: results from the National Women's Study.

    Science.gov (United States)

    Brewerton, Timothy D; Dansky, Bonnie S; O'Neil, Patrick M; Kilpatrick, Dean G

    2012-01-01

    Studies of birth patterns in anorexia nervosa have shown relative increases between March and August, while studies in Bulimia Nervosa (BN) have been negative. Since there are no studies using representative, nonclinical samples, we looked for seasonal birth patterns in women with BN and in those who ever endorsed bingeing or purging. A national, representative sample of 3,006 adult women completed structured telephone interviews including screenings for bulimia nervosa (BN) and questions about month, date, and year of birth. Season of birth was calculated using traditional definitions. Differences across season of birth between subjects with (n = 85) and without BN (n = 2,898), those with (n = 749) and without bingeing (n = 2,229), and those with (n = 267) and without any purging (n = 2,715) were compared using chi-square analyses. There were significant differences across season of birth between subjects: (1) with and without BN (p = 0.033); (2) with and without bingeing (p = 0.034), and; (3) with and without purging (p = 0.001). Fall had the highest relative number of births for all categories, while spring had the lowest. In a national representative study of nontreatment seeking subjects significant differences in season of birth were found for subjects with lifetime histories of BN, binge eating and purging. © 2011 by Wiley Periodicals, Inc. (Int J Eat Disord 2012). Copyright © 2011 Wiley Periodicals, Inc.

  3. Molecular purging of multiple myeloma cells by ex-vivo culture and retroviral transduction of mobilized-blood CD34+ cells

    Directory of Open Access Journals (Sweden)

    Corneo Gianmarco

    2007-07-01

    Full Text Available Abstract Background Tumor cell contamination of the apheresis in multiple myeloma is likely to affect disease-free and overall survival after autografting. Objective To purge myeloma aphereses from tumor contaminants with a novel culture-based purging method. Methods We cultured myeloma-positive CD34+ PB samples in conditions that retained multipotency of hematopoietic stem cells, but were unfavourable to survival of plasma cells. Moreover, we exploited the resistance of myeloma plasma cells to retroviral transduction by targeting the hematopoietic CD34+ cell population with a retroviral vector carrying a selectable marker (the truncated form of the human receptor for nerve growth factor, ΔNGFR. We performed therefore a further myeloma purging step by selecting the transduced cells at the end of the culture. Results Overall recovery of CD34+ cells after culture was 128.5%; ΔNGFR transduction rate was 28.8% for CD34+ cells and 0% for CD138-selected primary myeloma cells, respectively. Recovery of CD34+ cells after ΔNGFR selection was 22.3%. By patient-specific Ig-gene rearrangements, we assessed a decrease of 0.7–1.4 logs in tumor load after the CD34+ cell selection, and up to 2.3 logs after culture and ΔNGFR selection. Conclusion We conclude that ex-vivo culture and retroviral-mediated transduction of myeloma leukaphereses provide an efficient tumor cell purging.

  4. Análise de ácidos graxos não-esterificados de plasma humano por cromatografia gasosa capilar com injeção sem divisão de fluxo Analysis of non-esterified fatty acids in human plasma by capillary gas-chromatography with splitless injection

    Directory of Open Access Journals (Sweden)

    Jacqueline G. Ney

    2004-08-01

    Full Text Available The aim of the present work was to test the combination of non-esterified fatty acid (NEFA isolation using fumed silicon dioxide with capillary gas-chromatography (C-GC with splitless injection for the analysis of NEFAs in human plasma. Injection volume, solvent re-condensation and split purge flow-rate were the parameters evaluated for the analysis of fatty acid methyl esters by C-GC. The use of a solvent re-condensation technique, associated with 1.0 µL injection and a split purge flow rate of 80 mL/min resulted in satisfactory analysis of NEFAs. Fourteen fatty acids were identified in plasma samples, ranging from 2.03 to 184.0 µmol/L. The combination of both techniques proved useful for routine analyses of plasma NEFAs.

  5. Effects of slow recovery rates on water column geochemistry in aquitard wells

    Science.gov (United States)

    Schilling, K.E.

    2011-01-01

    Monitoring wells are often installed in aquitards to verify effectiveness for preventing migration of surface contaminants to underlying aquifers. However, water sampling of aquitard wells presents a challenge due to the slow recovery times for water recharging the wells, which can take as long as weeks, months or years to recharge depending on the sample volume needed. In this study, downhole profiling and sampling of aquitard wells was used to assess geochemical changes that occur in aquitard wells during water level recovery. Wells were sampled on three occasions spanning 11years, 1year and 1week after they were purged and casing water showed substantial water chemistry variations. Temperature decreased with depth, whereas pH and specific conductance increased with depth in the water column after 11years of water level recovery. Less stable parameters such as dissolved O2 (DO) and Eh showed strong zonation in the well column, with DO stratification occurring as the groundwater slowly entered the well. Oxidation of reduced till groundwater along with degassing of CO2 from till pore water affects mineral solubility and dissolved solid concentrations. Recommendations for sampling slowly recovering aquitard wells include identifying the zone of DO and Eh stratification in the well column and collecting water samples from below the boundary to better measure unstable geochemical parameters. ?? 2011 Elsevier Ltd.

  6. Investigation of the purging effect on a dead-end anode PEM fuel cell-powered vehicle during segments of a European driving cycle

    International Nuclear Information System (INIS)

    Gomez, Alberto; Sasmito, Agus P.; Shamim, Tariq

    2015-01-01

    Highlights: • Experimental study of a dead-end anode PEM fuel cell stack during a driving cycle. • Low purging duration is preferred at high current. • High purging frequency can sustain a better performance over time. • Lower cathode stoichiometry is preferred to minimize the parasitic loads. - Abstract: The dynamic performance of the PEM fuel cell is one of the key factors for successful operation of a fuel cell-powered vehicle. Maintaining fast time response while keeping stable and high stack performance is of importance, especially during acceleration and deceleration. In this paper, we evaluate the transient response of a PEM fuel cell stack with a dead-end anode during segments of a legislated European driving cycle together with the effect of purging factors. The PEM fuel cell stack comprises of 24 cells with a 300 cm"2 active catalyst area and operates at a low hydrogen and air pressure. Humidified air is supplied to the cathode side and the dry hydrogen is fed to the anode. The liquid coolant is circulated to the stack and the radiator to maintain the thermal envelope throughout the stack. The stack performance deterioration over time is prevented by utilizing the purging, which removes the accumulated water and impurities. The effect of purging period, purging duration, coolant flow rate and cathode stoichiometry are examined with regard to the fuel cell’s transient performance during the driving cycle. The results show that a low purging duration may avoid the undesired deceleration at a high current, and a high purging period may sustain a better performance over time. Moreover, the coolant flow rate is found to be an important parameter, which affects the stack temperature–time response of the cooling control and the stack performance, especially at high operating currents.

  7. Bridged polysilsesquioxane-based wide-bore monolithic capillary columns for hydrophilic interaction chromatography

    Czech Academy of Sciences Publication Activity Database

    Šesták, Jozef; Moravcová, Dana; Křenková, Jana; Planeta, Josef; Roth, Michal; Foret, František

    2017-01-01

    Roč. 1479, JAN (2017), s. 204-209 ISSN 0021-9673 R&D Projects: GA ČR(CZ) GA14-06319S; GA ČR(CZ) GA16-03749S Institutional support: RVO:68081715 Keywords : silica monolithic column * HILIC * oligosaccharides * nucleosides Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 3.981, year: 2016

  8. 3D capillary valves for versatile capillary patterning of channel walls

    NARCIS (Netherlands)

    Papadimitriou, Vasileios; van den Berg, Albert; Eijkel, Jan C.T.

    2016-01-01

    We demonstrate passive capillary patterning of channel walls with a liquid in situ. Patterning is performed using a novel 3D capillary valve system combining three standard capillary stop valves. A range of different patterns is demonstrated in three channel walls. Capillary patterning was designed

  9. Phosphatidylcholine covalently linked to a methacrylate-based monolith as a biomimetic stationary phase for capillary liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Carrasco-Correa, E. J.; Planeta, Josef; Lämmerhofer, M.; Wiedmer, S. K.

    2015-01-01

    Roč. 1402, JUL (2015), s. 27-35 ISSN 0021-9673 R&D Projects: GA MV VG20112015021 Institutional support: RVO:68081715 Keywords : Capillary LC * analyte–membrane interaction * monolithic column * phospholipids Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2015 http://hdl.handle.net/11104/0247268

  10. Kinetic modeling of the purging of activated carbon after short term methyl iodide loading

    International Nuclear Information System (INIS)

    Friedrich, V.; Lux, I.

    1991-01-01

    A bimolecular reaction model containing the physico-chemical parameters of the adsorption and desorption was developed earlier to describe the kinetics of methyl iodide retention by activated carbon adsorber. Both theoretical model and experimental investigations postulated constant upstream methyl iodide concentration till the maximum break-through. The work reported here includes the extension of the theoretical model to the general case when the concentration of the challenging gas may change in time. The effect of short term loading followed by purging with air, and an impulse-like increase in upstream gas concentration has been simulated. The case of short term loading and subsequent purging has been experimentally studied to validate the model. The investigations were carried out on non-impregnated activated carbon. A 4 cm deep carbon bed had been challenged by methyl iodide for 30, 90, 120 and 180 min and then purged with air, downstream methyl iodide concentration had been measured continuously. The main characteristics of the observed downstream concentration curves (time and slope of break-through, time and amplitude of maximum values) showed acceptable agreement with those predicted by the model

  11. Zwitterionic silica-based monolithic capillary columns for isocratic and gradient hydrophilic interaction liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Moravcová, Dana; Planeta, Josef; Kahle, Vladislav; Roth, Michal

    2012-01-01

    Roč. 1270, DEC 28 (2012), s. 178-185 ISSN 0021-9673 R&D Projects: GA MV VG20112015021; GA ČR(CZ) GAP206/11/0138; GA ČR(CZ) GAP106/12/0522 Institutional support: RVO:68081715 Keywords : HILIC * Monolithic silica column * Nucleoside separation * Nucleic acid base Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.612, year: 2012

  12. Application of a trap-free two-dimensional liquid chromatography combined with ion trap/time-of-flight mass spectrometry for separation and characterization of impurities and isomers in cefpiramide.

    Science.gov (United States)

    Wang, Jian; Xu, Yu; Wen, Chunmei; Wang, Zhijian

    2017-11-01

    High-resolution mass spectrometry had been routinely used for structure identification of impurity. However, all LC-MS methods were based on a volatile mobile phase, and a non-volatile system is used in the official analytical method of United States Pharmacopoeia for cefpiramide which limited the use of mass spectrometry for structure characterization of the impurities. Here we presented the utilization of a trap-free two-dimensional liquid chromatography coupled to high resolution ion trap/time-of-flight mass spectrometry (2D LC-IT-TOF MS) with positive and negative modes of electrospray ionization for characterization of eight impurities in cefpiramide. Trap-free two-dimensional liquid chromatography and online desalting technique made it possible to characterize the impurity in cefpiramide in the condition of official standard, and the TIC chromatogram of LC-MS was in conformity with the LC chromatogram of the official analytical method in the peak sequence of impurities, which could further improve the method of official monographs in pharmacopoeias. Each peak separated by the non-volatile mobile phase was trapped by a 20 μL quantitative loop then transferred into a system with a volatile mobile phase connected to a MS detector. In the first dimension, the column was Kromasil C 8 analytical column (250 mm × 4.6 mm, 5 μm) with a non-volatile salt mobile phase at the flow rate of 0.8 mL min -1 . In the second dimension, the column was Shimadzu Shim-pack GISS C 18 (50 mm × 2.1 mm, 1.9 μm) with a volatile salt mobile phase at the flow rate of 0.3 mL min -1 . Through the multiple heart-cutting 2D-LC approach and online desalting technique, the problem of incompatibility between non-volatile salt mobile phase and mass spectrometry was solved completely. The fragmentation behavior of cefpiramide and its eight impurities were studied. The structures of eight impurities in cefpiramide drug substance were deduced based on the HPLC-MS n data, in

  13. Non-radioactive determination of the penetration of methyl iodide through impregnated charcoals during dosing and purging

    International Nuclear Information System (INIS)

    Romans, J.B.; Deitz, V.R.

    1979-01-01

    A laboratory procedure is described using methyl iodide-127 which had the same linear flow of air (12.2 m/min) and contact time (0.25 sec.) as the RDT M16 Test Procedure. Only one-fourth of the charcoal was used (in a bed 2.54 cm diameter and 5.08 cm high) and the required dose of methyl iodide-127 was reduced from 5.25 to 1.31 mg. The inlet concentrations were determined with a gas chromatograph and the effluent concentrations with a modified microcoulombmeter. Two calibration procedures were used: (1) known vapor pressure of iodine crystals, and (2) quantitative pyrolysis of the methyl iodide-127 delivered from certified permeation tubes. Five charcoals and three impregnations were used in this study. Typical behaviors are given in 90% RH air with the charcoals either prehumidified for 16 hours at 90% RH or without the prehumidification. The breakthrough curves, concentration versus time, rose very slowly for the first 120 minutes and then more rapidly for an additional time. The lack of a dependence on the magnitude of the dose is compatible with a catalytic trapping mechanism. In the case of KI/sub x/ impregnations, there was excess emission of iodine during purging over that introduced as methyl iodide-127 which must have originated in the reservoir of iodine contained in the impregnation

  14. Purging of an air-filled vessel by horizontal injection of steam

    Energy Technology Data Exchange (ETDEWEB)

    Smith, B.L.; Andreani, M

    2000-07-01

    Reported here are results from an idealised 2D problem in which cold air is purged from a large vessel by a steam jet. The focus of the study is the prediction of the evolution of the flow regimes resulting from changes in the relative importance of buoyancy and inertia forces, and time histories of the temperature and concentration fields. Global parameters of interest are the mixture concentration at the vessel outlet and the total time taken to purge the air. The Computational Fluid Dynamics (CFD) code CFX-4 has been used to perform calculations for different inlet velocities, covering a range of (densimetric) Froude numbers from Fr=0.8 (buoyancy dominated) to Fr=7.1 (inertia dominated). Animations have been used to help understand the dynamics of the flow transitions, and temperature and concentration histories at specific monitoring points have been compared with coarse-mesh predictions obtained using the containment code GOTHIC. (authors)

  15. Purging of an air-filled vessel by horizontal injection of steam

    International Nuclear Information System (INIS)

    Smith, B.L.; Andreani, M.

    2000-01-01

    Reported here are results from an idealised 2D problem in which cold air is purged from a large vessel by a steam jet. The focus of the study is the prediction of the evolution of the flow regimes resulting from changes in the relative importance of buoyancy and inertia forces, and time histories of the temperature and concentration fields. Global parameters of interest are the mixture concentration at the vessel outlet and the total time taken to purge the air. The Computational Fluid Dynamics (CFD) code CFX-4 has been used to perform calculations for different inlet velocities, covering a range of (densimetric) Froude numbers from Fr=0.8 (buoyancy dominated) to Fr=7.1 (inertia dominated). Animations have been used to help understand the dynamics of the flow transitions, and temperature and concentration histories at specific monitoring points have been compared with coarse-mesh predictions obtained using the containment code GOTHIC. (authors)

  16. Methacrylate monolithic columns functionalized with epinephrine for capillary electrochromatography applications.

    Science.gov (United States)

    Carrasco-Correa, Enrique Javier; Ramis-Ramos, Guillermo; Herrero-Martínez, José Manuel

    2013-07-12

    Epinephrine-bonded polymeric monoliths for capillary electrochromatography (CEC) were developed by nucleophilic substitution reaction of epoxide groups of poly(glycidyl-methacrylate-co-ethylenedimethacrylate) (poly(GMA-co-EDMA)) monoliths using epinephrine as nucleophilic reagent. The ring opening reaction under dynamic conditions was optimized. Successful chemical modification of the monolith surface was ascertained by in situ Raman spectroscopy characterization. In addition, the amount of epinephrine groups that was bound to the monolith surface was evaluated by oxidation of the catechol groups with Ce(IV), followed by spectrophotometric measurement of unreacted Ce(IV). About 9% of all theoretical epoxide groups of the parent monolith were bonded to epinephrine. The chromatographic behavior of the epinephrine-bonded monolith in CEC conditions was assessed with test mixtures of alkyl benzenes, aniline derivatives and substituted phenols. In comparison to the poly(GMA-co-EDMA) monoliths, the epinephrine-bonded monoliths exhibited a much higher retention and slight differences in selectivity. The epinephrine-bonded monolith was further modified by oxidation with a Ce(IV) solution and compared with the epinephrine-bonded monoliths. The resulting monolithic stationary phases were evaluated in terms of reproducibility, giving RSD values below 9% in the parameters investigated. Copyright © 2013 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    Ren, Yu; Schlager, Hans; Martin, Damien

    2014-01-01

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

  18. Capillaries modified by noncovalent anionic polymer adsorption for capillary zone electrophoresis, micellar electrokinetic capillary chromatography and capillary electrophoresis mass spectrometry

    DEFF Research Database (Denmark)

    Bendahl, L; Hansen, S H; Gammelgaard, Bente

    2001-01-01

    A simple coating procedure for generation of a high and pH-independent electroosmotic flow in capillary zone electrophoresis (CZE) and micellar electrokinetic capillary chromatography (MEKC) is described. The bilayer coating was formed by noncovalent adsorption of the ionic polymers Polybrene...... capillaries was (4.9+/-0.1) x 10(-4) cm2V(-1)s(-1) in a pH-range of 2-10 (ionic strength = 30 mM). When alkaline compounds were used as test substances intracapillary and intercapillary migration time variations (n = 6) were less than 1% relative standard deviation (RSD) and 2% RSD, respectively in the entire...... pH range. The coating was fairly stable in the presence of sodium dodecyl sulfate, and this made it possible to perform fast MEKC separations at low pH. When neutral compounds were used as test substances, the intracapillary migration time variations (n = 6) were less than 2% RSD in a pH range of 2...

  19. Local area water removal analysis of a proton exchange membrane fuel cell under gas purge conditions.

    Science.gov (United States)

    Lee, Chi-Yuan; Lee, Yu-Ming; Lee, Shuo-Jen

    2012-01-01

    In this study, local area water content distribution under various gas purging conditions are experimentally analyzed for the first time. The local high frequency resistance (HFR) is measured using novel micro sensors. The results reveal that the liquid water removal rate in a membrane electrode assembly (MEA) is non-uniform. In the under-the-channel area, the removal of liquid water is governed by both convective and diffusive flux of the through-plane drying. Thus, almost all of the liquid water is removed within 30 s of purging with gas. However, liquid water that is stored in the under-the-rib area is not easy to remove during 1 min of gas purging. Therefore, the re-hydration of the membrane by internal diffusive flux is faster than that in the under-the-channel area. Consequently, local fuel starvation and membrane degradation can degrade the performance of a fuel cell that is started from cold.

  20. Needle trap extraction for GC analysis of formic and acetic acids in aqueous solution.

    Science.gov (United States)

    Lee, Xinqing; Huang, Daikuan; Lou, Dawei; Pawliszyn, Janusz

    2012-07-01

    Formic and acetic acids are ubiquitous in the environment, food, and most of the natural products. Extraction of the acids from aqueous solution is required for their isotope analysis by the gas chromatography-isotope ratio mass spectrometry. To this objective, we have previously developed a purge-and-trap technique using the dynamic solid-phase microextraction technology, the NeedlEX. The extraction efficiency, however, remains unexamined. Here, we address this question using the flame ionization detector and isotope ratio mass spectrometer while comparing it with that of the CAR/PDMS fiber. The results show that the NeedlEX is applicable at a wide range of concentration through coordination of purge volume given the minimum amount 3.7 ng and 1.8 ng of formic and acetic, respectively, is extracted. The efficiency of NeedlEX was 6-7 times lower than the fiber at 1000 μg/mL depending on the analyte. It is, however, superior to the latter at 10 μg/mL or less owing to its lower detection limit. The extraction efficiency of both acids is equivalent in molar amount. This is, however, disguised by the different response of the flame ionization detector. The isotope ratio mass spectrometor overcomes this problem but is compromised by relatively large errors. These results are particularly useful for isotopic analysis of carboxylic acids. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Hair analysis for illicit drugs by using capillary zone electrophoresis-electrospray ionization-ion trap mass spektrometry

    Czech Academy of Sciences Publication Activity Database

    Gottardo, R.; Bortolotti, F.; De Paoli, G.; Pascali, J. P.; Mikšík, Ivan; Tagliaro, F.

    2007-01-01

    Roč. 1159, 1-2 (2007), s. 185-189 ISSN 0021-9673 Institutional research plan: CEZ:AV0Z50110509 Keywords : capillary electrophoresis * hair analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.641, year: 2007

  2. Capillary Flow of Liquid Metals in Brazing

    Science.gov (United States)

    Dehsara, Mohammad

    Capillary flow is driven or controlled by capillary forces, exerted at the triple line where the fluid phases meet the solid boundary. Phase field (PF) models naturally accommodate diffusive triple line motion with variable contact angle, thus allowing for the no-slip boundary condition without the stress singularities. Moreover, they are uniquely suited for modeling of topological discontinuities which often arise during capillary flows. In this study, we consider diffusive triple line motion within two PF models: the compositionally compressible (CC) and the incompressible (IC) models. We derive the IC model as a systematic approximation to the CC model, based on a suitable choice of continuum velocity field. The CC model, applied to the fluids of dissimilar mass densities, exhibits a computational instability at the triple line. The IC model perfectly represents the analytic equilibria. We develop the parameter identification procedure and show that the triple line kinetics can be well represented by the IC model's diffusive boundary condition. The IC model is first tested by benchmarking the phase-field and experimental kinetics of water, and silicone oil spreading over the glass plates in which two systems do not interact with the substrate. Then, two high-temperature physical settings involving spreading of the molten Al-Si alloy: one over a rough wetting substrate, the other over a non-wetting substrate are modeled in a T-joint structure which is a typical geometric configuration for many brazing and soldering applications. Surface roughness directly influences the spreading of the molten metal by causing break-ups of the liquid film and trapping the liquid away from the joint. In the early stages of capillary flow over non-wetting surface, the melting and flow are concurrent, so that the kinetics of wetting is strongly affected by the variations in effective viscosity of the partially molten metal. We define adequate time-dependent functions for the

  3. Effect of nitrogen crossover on purging strategy in PEM fuel cell systems

    DEFF Research Database (Denmark)

    Rabbani, Raja Abid; Rokni, Masoud

    2013-01-01

    A comprehensive study on nitrogen crossover in polymer electrolyte membrane fuel cell (PEMFC) system with anode recirculation is conducted and associated purging strategies are discussed. Such systems when employed in automobiles are subjected to continuous changes in load and external operating...

  4. Fabrication of self-enclosed nanochannels based on capillary-pressure balance mechanism

    Science.gov (United States)

    Kou, Yu; Sang, Aixia; Li, Xin; Wang, Xudi

    2017-10-01

    Polymer-based micro/nano fluidic devices are becoming increasingly important to biological applications and fluidic control. In this paper, we propose a self-enclosure method for the fabrication of large-area nanochannels without external force by using a capillary-pressure balance mechanism. The melt polymer coated on the nanogrooves fills into the trenches inevitably and the air in the trenches is not excluded but compressed, which leads to an equilibrium state between pressure of the trapped air and capillary force of melt polymer eventually, resulting in the channels’ formation. A pressure balance model was proposed to elucidate the unique self-sealing phenomenon and the criteria for the design and construction of sealed channels was discussed. According to the bonding mechanism investigated using the volume of fluid (VOF) simulation and experiments, we can control the dimension of sealed channels by varying the baking condition. This fabrication technique has great potential for low-cost and mass production of polymeric-based micro/nano fluidic devices.

  5. Rapid improvements in emotion regulation predict intensive treatment outcome for patients with bulimia nervosa and purging disorder.

    Science.gov (United States)

    MacDonald, Danielle E; Trottier, Kathryn; Olmsted, Marion P

    2017-10-01

    Rapid and substantial behavior change (RSBC) early in cognitive behavior therapy (CBT) for eating disorders is the strongest known predictor of treatment outcome. Rapid change in other clinically relevant variables may also be important. This study examined whether rapid change in emotion regulation predicted treatment outcomes, beyond the effects of RSBC. Participants were diagnosed with bulimia nervosa or purging disorder (N = 104) and completed ≥6 weeks of CBT-based intensive treatment. Hierarchical regression models were used to test whether rapid change in emotion regulation variables predicted posttreatment outcomes, defined in three ways: (a) binge/purge abstinence; (b) cognitive eating disorder psychopathology; and (c) depression symptoms. Baseline psychopathology and emotion regulation difficulties and RSBC were controlled for. After controlling for baseline variables and RSBC, rapid improvement in access to emotion regulation strategies made significant unique contributions to the prediction of posttreatment binge/purge abstinence, cognitive psychopathology of eating disorders, and depression symptoms. Individuals with eating disorders who rapidly improve their belief that they can effectively modulate negative emotions are more likely to achieve a variety of good treatment outcomes. This supports the formal inclusion of emotion regulation skills early in CBT, and encouraging patient beliefs that these strategies are helpful. © 2017 Wiley Periodicals, Inc.

  6. A high-resolution non-invasive approach to quantify oxygen transport across the capillary fringe and within the underlying groundwater.

    Science.gov (United States)

    Haberer, Christina M; Rolle, Massimo; Liu, Sanheng; Cirpka, Olaf A; Grathwohl, Peter

    2011-03-25

    Oxygen transport across the capillary fringe is relevant for many biogeochemical processes. We present a non-invasive technique, based on optode technology, to measure high-resolution concentration profiles of oxygen across the unsaturated/saturated interface. By conducting a series of quasi two-dimensional flow-through laboratory experiments, we show that vertical hydrodynamic dispersion in the water-saturated part of the capillary fringe is the process limiting the mass transfer of oxygen. A number of experimental conditions were tested in order to investigate the influence of grain size and horizontal flow velocity on transverse vertical dispersion in the capillary fringe. In the same setup, analogous experiments were simultaneously carried out in the fully water-saturated zone, therefore allowing a direct comparison with oxygen transfer across the capillary fringe. The outcomes of the experiments under various conditions show that oxygen transport in the two zones of interest (i.e., the unsaturated/saturated interface and the saturated zone) is characterized by very similar transverse dispersion coefficients. An influence of the capillary fringe morphology on oxygen transport has not been observed. These results may be explained by the narrow grain size distribution used in the experiments, leading to a steep decline in water saturation at the unsaturated/saturated interface and to the absence of trapped gas in this transition zone. We also modeled flow (applying the van Genuchten and the Brooks-Corey relationships) and two-dimensional transport across the capillary fringe, obtaining simulated profiles of equivalent aqueous oxygen concentration that were in good agreement with the observations. Copyright © 2010 Elsevier B.V. All rights reserved.

  7. Motion of liquid plugs between vapor bubbles in capillary tubes: a comparison between fluids

    Science.gov (United States)

    Bertossi, Rémi; Ayel, Vincent; Mehta, Balkrishna; Romestant, Cyril; Bertin, Yves; Khandekar, Sameer

    2017-11-01

    Pulsating heat pipes (PHP) are now well-known devices in which liquid/vapor slug flow oscillates in a capillary tube wound between hot and cold sources. In this context, this paper focuses on the motion of the liquid plug, trapped between vapor bubbles, moving in capillary tubes, to try to better understand the thermo-physical phenomena involved in such devices. This study is divided into three parts. In the first part, an experimental study presents the evolution of the vapor pressure during the evaporation process of a liquid thin film deposited from a liquid plug flowing in a heated capillary tube: it is found that the behavior of the generated and removed vapor can be very different, according to the thermophysical properties of the fluids. In the second part, a transient model allows to compare, in terms of pressure and duration, the motion of a constant-length liquid plug trapped between two bubbles subjected to a constant difference of vapor pressure: the results highlight that the performances of the four fluids are also very different. Finally, a third model that can be considered as an improvement of the second one, is also presented: here, the liquid slug is surrounded by two vapor bubbles, one subjected to evaporation, the pressure in both bubbles is now a result of the calculation. This model still allows comparing the behaviors of the fluid. Even if our models are quite far from a complete model of a real PHP, results do indicate towards the applicability of different fluids as suitable working fluids for PHPs, particularly in terms of the flow instabilities which they generate.

  8. An investigation of the joint longitudinal trajectories of low body weight, binge eating, and purging in women with anorexia nervosa and bulimia nervosa

    Science.gov (United States)

    Lavender, Jason M.; De Young, Kyle P.; Franko, Debra L.; Eddy, Kamryn T.; Kass, Andrea E.; Sears, Meredith S.; Herzog, David B.

    2015-01-01

    Objectives To describe the longitudinal course of three core eating disorder symptoms – low body weight, binge eating, and purging – in women with anorexia nervosa (AN) and bulimia nervosa (BN) using a novel statistical approach. Method Treatment-seeking women with AN (n=136) or BN (n=110) completed the Eating Disorders Longitudinal Interval Follow-Up Evaluation interview every six months, yielding weekly eating disorder symptom data for a five-year period. Semi-parametric mixture modeling was used to identify longitudinal trajectories for the three core symptoms. Results Four individual trajectories were identified for each eating disorder symptom. The number and general shape of the individual trajectories was similar across symptoms, with each model including trajectories depicting stable absence and stable presence of symptoms as well as one or more trajectories depicting the declining presence of symptoms. Unique trajectories were found for low body weight (fluctuating presence) and purging (increasing presence). Conjunction analyses yielded the following joint trajectories: low body weight and binge eating, low body weight and purging, and binge eating and purging. Conclusions The course of individual eating disorder symptoms among patients with AN and BN is highly variable. Future research identifying clinical predictors of trajectory membership may inform treatment and nosological research. PMID:22072404

  9. An investigation of the joint longitudinal trajectories of low body weight, binge eating, and purging in women with anorexia nervosa and bulimia nervosa.

    Science.gov (United States)

    Lavender, Jason M; De Young, Kyle P; Franko, Debra L; Eddy, Kamryn T; Kass, Andrea E; Sears, Meredith S; Herzog, David B

    2011-12-01

    To describe the longitudinal course of three core eating disorder symptoms-low body weight, binge eating, and purging-in women with anorexia nervosa (AN) and bulimia nervosa (BN) using a novel statistical approach. Treatment-seeking women with AN (n = 136) or BN (n = 110) completed the Eating Disorders Longitudinal Interval Follow-Up Evaluation interview every 6 months, yielding weekly eating disorder symptom data for a 5-year period. Semiparametric mixture modeling was used to identify longitudinal trajectories for the three core symptoms. Four individual trajectories were identified for each eating disorder symptom. The number and general shape of the individual trajectories was similar across symptoms, with each model including trajectories depicting stable absence and stable presence of symptoms as well as one or more trajectories depicting the declining presence of symptoms. Unique trajectories were found for low body weight (fluctuating presence) and purging (increasing presence). Conjunction analyses yielded the following joint trajectories: low body weight and binge eating, low body weight and purging, and binge eating and purging. The course of individual eating disorder symptoms among patients with AN and BN is highly variable. Future research identifying clinical predictors of trajectory membership may inform treatment and nosological research. Copyright © 2010 Wiley Periodicals, Inc.

  10. Less symptomatic, but equally impaired: Clinical impairment in restricting versus binge-eating/purging subtype of anorexia nervosa.

    Science.gov (United States)

    Reas, Deborah Lynn; Rø, Øyvind

    2018-01-01

    This study investigated subtype differences in eating disorder-specific impairment in a treatment-seeking sample of individuals with anorexia nervosa (AN). The Clinical Impairment Assessment (CIA) and the Eating Disorder Examination-Questionnaire (EDE-Q) were administered to 142 patients. Of these, 54.9% were classified as restricting type (AN-R) and 45.1% were classified as binge-eating/purging type (AN-B/P) based on an average weekly occurrence of binge eating and/or purging episodes (≥4 episodes/28days). Individuals with AN-B/P exhibited higher levels of core ED psychopathology (dietary restraint, eating concern, shape/weight concerns) in addition to the expected higher frequency of binge/purge episodes. No significant differences existed between AN subtypes in the severity of ED-related impairment. Weight/shape concerns and binge eating frequency significantly predicted level of impairment. Differential associations were observed between the type of ED pathology that significantly contributed to impairment according to AN subtype. Although those with AN-B/P displayed higher levels of core attitudinal and behavioral ED pathology than AN-R, no significant differences in ED-specific impairment were found between AN subtypes. Eating disorder-related impairment in AN was not related to the severity of underweight or purging behaviors, but was uniquely and positively associated with weight/shape concerns and binge eating frequency. Copyright © 2018 Elsevier Ltd. All rights reserved.

  11. A complete soil hydraulic model accounting for capillary and adsorptive water retention, capillary and film conductivity, and hysteresis

    NARCIS (Netherlands)

    Sakai, Masaru; Van Genuchten, Martinus Th|info:eu-repo/dai/nl/31481518X; Alazba, A. A.; Setiawan, Budi Indra; Minasny, Budiman

    2015-01-01

    A soil hydraulic model that considers capillary hysteretic and adsorptive water retention as well as capillary and film conductivity covering the complete soil moisture range is presented. The model was obtained by incorporating the capillary hysteresis model of Parker and Lenhard into the hydraulic

  12. Multiple capillary biochemical analyzer

    Science.gov (United States)

    Dovichi, N.J.; Zhang, J.Z.

    1995-08-08

    A multiple capillary analyzer allows detection of light from multiple capillaries with a reduced number of interfaces through which light must pass in detecting light emitted from a sample being analyzed, using a modified sheath flow cuvette. A linear or rectangular array of capillaries is introduced into a rectangular flow chamber. Sheath fluid draws individual sample streams through the cuvette. The capillaries are closely and evenly spaced and held by a transparent retainer in a fixed position in relation to an optical detection system. Collimated sample excitation radiation is applied simultaneously across the ends of the capillaries in the retainer. Light emitted from the excited sample is detected by the optical detection system. The retainer is provided by a transparent chamber having inward slanting end walls. The capillaries are wedged into the chamber. One sideways dimension of the chamber is equal to the diameter of the capillaries and one end to end dimension varies from, at the top of the chamber, slightly greater than the sum of the diameters of the capillaries to, at the bottom of the chamber, slightly smaller than the sum of the diameters of the capillaries. The optical system utilizes optic fibers to deliver light to individual photodetectors, one for each capillary tube. A filter or wavelength division demultiplexer may be used for isolating fluorescence at particular bands. 21 figs.

  13. Effect of capillary forces on immiscible two-phase flow in heterogeneous porous media

    Energy Technology Data Exchange (ETDEWEB)

    van Duijn, C.J.; Molenaar, J.; de Neef, M.J.

    1994-12-31

    We consider the one-dimensional two-phase flow including capillary effects through a heterogeneous porous medium. The heterogeneity is due to the spatial variation of the absolute permeability and the porosity. Both these quantities are assumed to be piecewise constant. At interfaces where the rock properties are discontinuous, we derive, by a regularization technique, conditions to match the values of the saturation on both sides. There are two conditions: a flux condition and an extended pressure condition. Applying these conditions we show that trapping of the wetting phase may occur near hetergeneities. To illustrate the behavior of the saturation we consider a time-dependent diffusion problem without convection, a stationary convection-diffusion problem, and the full time-dependent convection-diffusion problem (numerically). In particular the last two problems explicitly show the trapping behavior.

  14. Investigation of the output pulse characteristics of a 46.9 nm Ar capillary discharge soft x-ray laser

    International Nuclear Information System (INIS)

    Ritucci, A.; Tomassetti, G.; Palladino, L.; Reale, A.; Gaeta, G.; Limongi, T.; Flora, F.; Mezi, L.; Kukhlevsky, S.V.; Kaiser, J.; Faenov, A.; Pikuz, T.; Reale, L.

    2002-01-01

    In this paper, we report on the realization of a capillary discharge soft x-ray laser operating at 46.9 nm pumped by a 30 kA peak value, 150 ns half cycle duration current pulse (corresponding to a mean current slope of about 5 1011 A/s). The slope of the pumping current is sufficiently high to produce the plasma compression and laser amplification on the 3p-3s, J=0-1 transition of Ne-like Ar, in 2.4-4 mm in diameter alumina capillary channels. We have analyzed the output pulse characteristics of the produced laser beam, such as the lasing time and the pulse duration, the saturation and the output pulse energy, the near field image as a function of different experimental parameters. Using the same current pulse, the lasing effect has not been observed in polyacetal capillaries, demonstrating the damning role of the wall capillary ablation in the heating and in the stability of the plasma column during the z-pinch compression

  15. Study of typical nuclear containment purge valves in an accident environment

    International Nuclear Information System (INIS)

    Watkins, J.C.; Steele, R. Jr.; Hill, R.C.; DeWall, K.G.

    1986-08-01

    This report presents the results of the containment purge and vent valve test program, conducted under the sponsorship of the United States Nuclear Regulatory Commission (NRC), Office of Nuclear Regulatory Research. The test program investigated butterfly valve operability and leak integrity under light-water-reactor design basis and severe accident conditions. Three nuclear-designed butterfly valves typical of those used in domestic nuclear power plant containment purge and vent applications were tested. For a comparison of response, two valve of the same size with differing internal designs were tested. For extrapolation insights, a larger-sized valve similar to one of the smaller valves was also tested. Dynamic flow tests were performed over the range of design basis accident pressures. Leak integrity testing was also performed at both design basis and severe accident temperatures and pressures. The valve experiments were performed with various piping configurations and valve orientations to the flow to simulate the various installation options in field applications. Testing was also performed in a standard ANSI test section

  16. In-well time-of-travel approach to evaluate optimal purge duration during low-flow sampling of monitoring wells

    Science.gov (United States)

    Harte, Philip T.

    2017-01-01

    A common assumption with groundwater sampling is that low (time until inflow from the high hydraulic conductivity part of the screened formation can travel vertically in the well to the pump intake. Therefore, the length of the time needed for adequate purging prior to sample collection (called optimal purge duration) is controlled by the in-well, vertical travel times. A preliminary, simple analytical model was used to provide information on the relation between purge duration and capture of formation water for different gross levels of heterogeneity (contrast between low and high hydraulic conductivity layers). The model was then used to compare these time–volume relations to purge data (pumping rates and drawdown) collected at several representative monitoring wells from multiple sites. Results showed that computation of time-dependent capture of formation water (as opposed to capture of preexisting screen water), which were based on vertical travel times in the well, compares favorably with the time required to achieve field parameter stabilization. If field parameter stabilization is an indicator of arrival time of formation water, which has been postulated, then in-well, vertical flow may be an important factor at wells where low-flow sampling is the sample method of choice.

  17. Ion guiding and losses in insulator capillaries

    International Nuclear Information System (INIS)

    Juhasz, Z.; Sulik, B.; Vikor, Gy.; Biri, S.; Fekete, E.; Ivan, I.; Gall, F.; Toekesi, K.; Matefi-Tempfli, S.; Matefi-Tempfli, M.

    2007-01-01

    Complete text of publication follows. Not long ago it was discovered that insulating capillaries can guide slow ions, so that the ions avoid close contact with the capillary walls and preserve their initial charge state. This phenomenon did not only give a new puzzle for theoreticians but opened the way for new possible applications where ions are manipulated (deflected, focused and directed to different patterns on the irradiated media) with small capillary devices. The most important question for such applications is how large fraction of the ions can be guided to the desired direction. It is already known that the ion guiding is due to the charging up of the inner capillary walls by earlier ion impact events. In tilted capillaries one side of the capillary walls charges up. This deflects the later arriving ions, so that some of them pass through the capillaries nearly parallel with respect to their axes. The angle where the transmission drops to 1/e of the direct transmission at 0 deg is the guiding angle, which characterize the guiding ability. At 0 deg the ideal 100 percent transmission for the ions, which enter the capillaries, is reduced due to the mirror charge attraction and geometrical imperfections. These losses appear in the transmission for tilted capillaries with similar magnitude, since after the deflection region, which usually restricted to the close surroundings of the capillary openings, the guided ions pass through the rest of the capillaries as in non-tilted samples. In our experimental studies with Al 2 O 3 capillaries we found that around 90 percent of the incoming ions are lost. To understand these significant losses, the effects of the mirror charge attraction and geometrical imperfections have been calculated classically. The mirror charge potential was taken from.The model of the capillaries used in the calculations can be seen in Figure 1. The calculations have shown that the effects of mirror charge attraction and the angular

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

    Science.gov (United States)

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

    2018-05-15

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

  19. Optical trapping and binding of particles in an optofluidic stable Fabry-Pérot resonator with single-sided injection.

    Science.gov (United States)

    Gaber, Noha; Malak, Maurine; Marty, Frédéric; Angelescu, Dan E; Richalot, Elodie; Bourouina, Tarik

    2014-07-07

    In this article, microparticles are manipulated inside an optofluidic Fabry-Pérot cylindrical cavity embedding a fluidic capillary tube, taking advantage of field enhancement and multiple reflections within the optically-resonant cavity. This enables trapping of suspended particles with single-side injection of light and with low optical power. A Hermite-Gaussian standing wave is developed inside the cavity, forming trapping spots at the locations of the electromagnetic field maxima with a strong intensity gradient. The particles get arranged in a pattern related to the mechanism affecting them: either optical trapping or optical binding. This is proven to eventually translate into either an axial one dimensional (1D) particle array or a cluster of particles. Numerical simulations are performed to model the field distributions inside the cavity allowing a behavioral understanding of the phenomena involved in each case.

  20. Does haplodiploidy purge inbreeding depression in rotifer populations?

    Directory of Open Access Journals (Sweden)

    Ana M Tortajada

    2009-12-01

    Full Text Available Inbreeding depression is an important evolutionary factor, particularly when new habitats are colonized by few individuals. Then, inbreeding depression by drift could favour the establishment of later immigrants because their hybrid offspring would enjoy higher fitness. Rotifers are the only major zooplanktonic group where information on inbreeding depression is still critically scarce, despite the fact that in cyclical parthenogenetic rotifers males are haploid and could purge deleterious recessive alleles, thereby decreasing inbreeding depression.We studied the effects of inbreeding in two populations of the cyclical parthenogenetic rotifer Brachionus plicatilis. For each population, we compared both the parental fertilization proportion and F1 fitness components from intraclonal (selfed and interclonal (outcrossed crosses. The parental fertilization proportion was similar for both types of crosses, suggesting that there is no mechanism to avoid selfing. In the F1 generation of both populations, we found evidence of inbreeding depression for the fitness components associated with asexual reproduction; whereas inbreeding depression was only found for one of the two sexual reproduction fitness components measured.Our results show that rotifers, like other major zooplanktonic groups, can be affected by inbreeding depression in different stages of their life cycle. These results suggest that haplodiploidy does not purge efficiently deleterious recessive alleles. The inbreeding depression detected here has important implications when a rotifer population is founded and intraclonal crossing is likely to occur. Thus, during the foundation of new populations inbreeding depression may provide opportunities for new immigrants, increasing gene flow between populations, and affecting genetic differentiation.

  1. Does Haplodiploidy Purge Inbreeding Depression in Rotifer Populations?

    Science.gov (United States)

    Tortajada, Ana M.; Carmona, María José; Serra, Manuel

    2009-01-01

    Background Inbreeding depression is an important evolutionary factor, particularly when new habitats are colonized by few individuals. Then, inbreeding depression by drift could favour the establishment of later immigrants because their hybrid offspring would enjoy higher fitness. Rotifers are the only major zooplanktonic group where information on inbreeding depression is still critically scarce, despite the fact that in cyclical parthenogenetic rotifers males are haploid and could purge deleterious recessive alleles, thereby decreasing inbreeding depression. Methodology/Principal Findings We studied the effects of inbreeding in two populations of the cyclical parthenogenetic rotifer Brachionus plicatilis. For each population, we compared both the parental fertilization proportion and F1 fitness components from intraclonal (selfed) and interclonal (outcrossed) crosses. The parental fertilization proportion was similar for both types of crosses, suggesting that there is no mechanism to avoid selfing. In the F1 generation of both populations, we found evidence of inbreeding depression for the fitness components associated with asexual reproduction; whereas inbreeding depression was only found for one of the two sexual reproduction fitness components measured. Conclusions/Significance Our results show that rotifers, like other major zooplanktonic groups, can be affected by inbreeding depression in different stages of their life cycle. These results suggest that haplodiploidy does not purge efficiently deleterious recessive alleles. The inbreeding depression detected here has important implications when a rotifer population is founded and intraclonal crossing is likely to occur. Thus, during the foundation of new populations inbreeding depression may provide opportunities for new immigrants, increasing gene flow between populations, and affecting genetic differentiation. PMID:19997616

  2. Capillary leak syndrome: etiologies, pathophysiology, and management.

    Science.gov (United States)

    Siddall, Eric; Khatri, Minesh; Radhakrishnan, Jai

    2017-07-01

    In various human diseases, an increase in capillary permeability to proteins leads to the loss of protein-rich fluid from the intravascular to the interstitial space. Although sepsis is the disease most commonly associated with this phenomenon, many other diseases can lead to a "sepsis-like" syndrome with manifestations of diffuse pitting edema, exudative serous cavity effusions, noncardiogenic pulmonary edema, hypotension, and, in some cases, hypovolemic shock with multiple-organ failure. The term capillary leak syndrome has been used to describe this constellation of disease manifestations associated with an increased capillary permeability to proteins. Diseases other than sepsis that can result in capillary leak syndrome include the idiopathic systemic capillary leak syndrome or Clarkson's disease, engraftment syndrome, differentiation syndrome, the ovarian hyperstimulation syndrome, hemophagocytic lymphohistiocytosis, viral hemorrhagic fevers, autoimmune diseases, snakebite envenomation, and ricin poisoning. Drugs including some interleukins, some monoclonal antibodies, and gemcitabine can also cause capillary leak syndrome. Acute kidney injury is commonly seen in all of these diseases. In addition to hypotension, cytokines are likely to be important in the pathophysiology of acute kidney injury in capillary leak syndrome. Fluid management is a critical part of the treatment of capillary leak syndrome; hypovolemia and hypotension can cause organ injury, whereas capillary leakage of administered fluid can worsen organ edema leading to progressive organ injury. The purpose of this article is to discuss the diseases other than sepsis that produce capillary leak and review their collective pathophysiology and treatment. Copyright © 2017 International Society of Nephrology. Published by Elsevier Inc. All rights reserved.

  3. Gas-Filled Capillary Model

    International Nuclear Information System (INIS)

    Steinhauer, L. C.; Kimura, W. D.

    2006-01-01

    We have developed a 1-D, quasi-steady-state numerical model for a gas-filled capillary discharge that is designed to aid in selecting the optimum capillary radius in order to guide a laser beam with the required intensity through the capillary. The model also includes the option for an external solenoid B-field around the capillary, which increases the depth of the parabolic density channel in the capillary, thereby allowing for propagation of smaller laser beam waists. The model has been used to select the parameters for gas-filled capillaries to be utilized during the Staged Electron Laser Acceleration -- Laser Wakefield (STELLA-LW) experiment

  4. Simple, specific analysis of organophosphorus and carbamate pesticides in sediments using column extraction and gas chromatography

    Science.gov (United States)

    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.

  5. Krohne Flow Indicator and High Flow Alarm - Local Indicator and High Flow Alarm of Helium Flow from the SCHe Purge Lines C and D to the Process Vent

    International Nuclear Information System (INIS)

    MISKA, C.R.

    2000-01-01

    Flow Indicators/alarms FI/FSH-5*52 and -5*72 are located in the process vent lines connected to the 2 psig SCHe purge lines C and D. They monitor the flow from the 2 psig SCHe purge going to the process vent. The switch/alarm is non-safety class GS

  6. Analysis of volatile headspace gases sampled by cryogenic traps from Westinghouse Hanford Company Tank 242-C-112 March 1992

    International Nuclear Information System (INIS)

    Lucke, R.B.; Clauss, S.A.

    1993-10-01

    Results are given from gas chromatography/mass spectrometry (GC/MS) analyses of the headspace samples obtained by using cryogenic traps from Westinghouse Hanford Company (WHC) Tank 112-C during the month of March, 1992. Samples were analyzed as received with no sample preparation. Analyses included direct GC/MS for volatile/semivolatile components, and direct GC/MS for ammonia. Purge and trap GC/MS analysis was not done. In addition, aliquots were sent to Karl Pool, Pacific Northwest Laboratory, for hydrogen cyanide analysis by ion chromatography, the results are reported here. All concentrations are reported for the methanol extract solutions. To calculate concentrations in the headspace, the cryo-sampling air volume and the methanol rinse volume must be obtained from cryo-sampling personnel at WHC. Triplicate analyses were done on all samples, and average concentrations and standard deviations are reported. One significant result was that no ammonia was detected

  7. Capillaries for use in a multiplexed capillary electrophoresis system

    Science.gov (United States)

    Yeung, E.S.; Chang, H.T.; Fung, E.N.

    1997-12-09

    The invention provides a side-entry optical excitation geometry for use in a multiplexed capillary electrophoresis system. A charge-injection device is optically coupled to capillaries in the array such that the interior of a capillary is imaged onto only one pixel. In Sanger-type 4-label DNA sequencing reactions, nucleotide identification (``base calling``) is improved by using two long-pass filters to split fluorescence emission into two emission channels. A binary poly(ethyleneoxide) matrix is used in the electrophoretic separations. 19 figs.

  8. Capillary detectors

    International Nuclear Information System (INIS)

    Konijn, J.; Winter, K.; Vilain, P.; Wilquet, G.; Fabre, J.P.; Kozarenko, E.; Kreslo, I.; Goldberg, J.; Hoepfner, K.; Bay, A.; Currat, C.; Koppenburg, P.; Frekers, D.; Wolff, T.; Buontempo, S.; Ereditato, A.; Frenkel, A.; Liberti, B.; Martellotti, G.; Penso, G.; Ekimov, A.; Golovkin, S.; Govorun, V.; Medvedkov, A.; Vasil'chenko, V.

    1998-01-01

    The option for a microvertex detector using glass capillary arrays filled with liquid scintillator is presented. The status of capillary layers development and possible read-out techniques for high rate environment are reported. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

  9. Nonlinear PIC simulation in a Penning trap

    International Nuclear Information System (INIS)

    Lapenta, G.; Delzanno, G.L.; Finn, J. M.

    2002-01-01

    We study the nonlinear dynamics of a Penning trap plasma, including the effect of the finite length and end curvature of the plasma column. A new cylindrical PIC code, called KANDINSKY, has been implemented by using a new interpolation scheme. The principal idea is to calculate the volume of each cell from a particle volume, in the same manner as it is done for the cell charge. With this new method, the density is conserved along streamlines and artificial sources of compressibility are avoided. The code has been validated with a reference Eulerian fluid code. We compare the dynamics of three different models: a model with compression effects, the standard Euler model and a geophysical fluid dynamics model. The results of our investigation prove that Penning traps can really be used to simulate geophysical fluids

  10. Highly crosslinked polymeric monoliths for reversed-phase capillary liquid chromatography of small molecules.

    Science.gov (United States)

    Liu, Kun; Tolley, H Dennis; Lee, Milton L

    2012-03-02

    Seven crosslinking monomers, i.e., 1,3-butanediol dimethacrylate (1,3-BDDMA), 1,4-butanediol dimethacrylate (1,4-BDDMA), neopentyl glycol dimethacrylate (NPGDMA), 1,5-pentanediol dimethacrylate (1,5-PDDMA), 1,6-hexanediol dimethacrylate (1,6-HDDMA), 1,10-decanediol dimethacrylate (1,10-DDDMA), and 1,12-dodecanediol dimethacrylate (1,12-DoDDMA), were used to synthesize highly cross-linked monolithic capillary columns for reversed-phase liquid chromatography (RPLC) of small molecules. Dodecanol and methanol were chosen as "good" and "poor" porogenic solvents, respectively, for these monoliths, and were investigated in detail to provide insight into the selection of porogen concentration using 1,12-DoDDMA. Isocratic elution of alkylbenzenes at a flow rate of 300 nL/min was conducted for all of the monoliths. Gradient elution of alkylbenzenes and alkylparabens provided high resolution separations. Optimized monoliths synthesized from all seven crosslinking monomers showed high permeability. Several of the monoliths demonstrated column efficiencies in excess of 50,000 plates/m. Monoliths with longer alkyl-bridging chains showed very little shrinking or swelling in solvents of different polarities. Column preparation was highly reproducible; the relative standard deviation (RSD) values (n=3) for run-to-run and column-to-column were less than 0.25% and 1.20%, respectively, based on retention times of alkylbenzenes. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Urea functionalized surface-bonded sol-gel coating for on-line hyphenation of capillary microextraction with high-performance liquid chromatography.

    Science.gov (United States)

    Jillani, Shehzada Muhammad Sajid; Alhooshani, Khalid

    2018-03-30

    Sol-gel urea functionalized-[bis(hydroxyethyl)amine] terminated polydimethylsiloxane coating was developed for capillary microextraction-high performance liquid chromatographic analysis from aqueous samples. A fused silica capillary is coated from the inside with surface bonded coating material and is created through in-situ sol-gel reaction. The urea-functionalized coating was immobilized to the inner surface of the capillary by the condensation reaction of silanol groups of capillary and sol-solution. The characterization of the coating material was successfully done by using X-ray photoelectron spectroscopy, thermogravimetric analysis, field emission scanning electron microscope, and energy dispersive X-ray spectrometer. To make a setup of online capillary microextraction-high performance liquid chromatography, the urea functionalized capillary was installed in the HPLC manual injection port. The analytes of interest were pre-concentrated in the coated sampling loop, desorbed by the mobile phase, chromatographically separated on C-18 column, and analyzed by UV detector. Sol-gel coated capillaries were used for online extraction and high-performance liquid chromatographic analysis of phenols, ketones, aldehydes, and polyaromatic hydrocarbons. This newly developed coating showed excellent extraction for a variety of analytes ranging from highly polar to non-polar in nature. The analysis using sol-gel coating showed excellent overall sensitivity in terms of lower detection limits (S/N = 3) for the analytes (0.10 ng mL -1 -14.29 ng mL -1 ) with acceptable reproducibility that is less than 12.0%RSD (n = 3). Moreover, the capillary to capillary reproducibility of the analysis was also tested by changing the capillary of the same size. This provided excellent%RSD of less than 10.0% (n = 3). Copyright © 2018 Elsevier B.V. All rights reserved.

  12. The kinetics of hydrogen removal from liquid sodium

    International Nuclear Information System (INIS)

    Gwyther, J.R.; Whittingham, A.C.

    1981-01-01

    The rates of hydrogen removal from liquid sodium-sodium hydride mixtures have been measured as a function of sodium stirring rate at temperatures up to 420 0 C. Two techniques have been employed - removal under continuous evacuation in which hydrogen flow rates were measured using a capillary flow technique and by argon purging in which hydrogen concentrations in the argon carrier gas were measured by gas chromatography. The results have been used to assess the feasibility of thermal decomposition of sodium hydride for the regeneration of hydride-laden LMFBR cold traps. Studies on the kinetics of desorption of hydrogen from solution in liquid sodium at temperatures up to 400 0 C are also presented and possible kinetic mechanisms discussed. (orig.)

  13. Absorption column working study for iodine formed in spent fuel reprocessing plant gaseous effluents: hydrodynamic and mass transfer

    International Nuclear Information System (INIS)

    Vignau, B.

    1986-09-01

    The hydrodynamic and matter transfer parameters has been studied on absorption columns destined to trap iodine issued of spent fuel reprocessing plants. These columns have different packing - Raschig rings (glass, ceramic, PVC, steel) - Berl saddles (ceramic) - Weaved metallic thread (steel). The effect of dimension and of packing structure on gas pressure drop and on liquid holdup has been evaluated. The partial transfer coefficients of I 2 -Air-NaOH system has been the object of an experimental study. This system can be simulated by CO 2 -Air-NaOH system [fr

  14. Evaluation of the Validity of Groundwater Samples Obtained Using the Purge Water Management System at SRS

    International Nuclear Information System (INIS)

    Beardsley, C.C.

    1999-01-01

    As part of the demonstration testing of the Purge Water Management System (PWMS) technology at the Savannah River Site (SRS), four wells were equipped with PWMS units in 1997 and a series of sampling events were conducted at each during 1997-1998. Three of the wells were located in A/M Area while the fourth was located at the Old Radioactive Waste Burial Ground in the General Separations Area.The PWMS is a ''closed-loop'', non-contact, system used to collect and return purge water to the originating aquifer after a sampling event without having significantly altered the water quality. One of the primary concerns as to its applicability at SRS, and elsewhere, is whether the PWMS might resample groundwater that is returned to the aquifer during the previous sampling event. The purpose of the present investigation was to compare groundwater chemical analysis data collected at the four test wells using the PWMS vs. historical data collected using the standard monitoring program methodology to determine if the PWMS provides representative monitoring samples.The analysis of the groundwater chemical concentrations indicates that the PWMS sampling methodology acquired representative groundwater samples at monitoring wells ABP-1A, ABP-4, ARP-3 and BGO-33C. Representative groundwater samples are achieved if the PWMS does not resample groundwater that has been purged and returned during a previous sampling event. Initial screening calculations, conducted prior to the selection of these four wells, indicated that groundwater velocities were high enough under the ambient hydraulic gradients to preclude resampling from occurring at the time intervals that were used at each well. Corroborating evidence included a tracer test that was conducted at BGO-33C, the high degree of similarity between analyte concentrations derived from the PWMS samples and those obtained from historical protocol sampling, as well as the fact that PWMS data extend all previously existing concentration

  15. Automated Parallel Capillary Electrophoretic System

    Science.gov (United States)

    Li, Qingbo; Kane, Thomas E.; Liu, Changsheng; Sonnenschein, Bernard; Sharer, Michael V.; Kernan, John R.

    2000-02-22

    An automated electrophoretic system is disclosed. The system employs a capillary cartridge having a plurality of capillary tubes. The cartridge has a first array of capillary ends projecting from one side of a plate. The first array of capillary ends are spaced apart in substantially the same manner as the wells of a microtitre tray of standard size. This allows one to simultaneously perform capillary electrophoresis on samples present in each of the wells of the tray. The system includes a stacked, dual carousel arrangement to eliminate cross-contamination resulting from reuse of the same buffer tray on consecutive executions from electrophoresis. The system also has a gel delivery module containing a gel syringe/a stepper motor or a high pressure chamber with a pump to quickly and uniformly deliver gel through the capillary tubes. The system further includes a multi-wavelength beam generator to generate a laser beam which produces a beam with a wide range of wavelengths. An off-line capillary reconditioner thoroughly cleans a capillary cartridge to enable simultaneous execution of electrophoresis with another capillary cartridge. The streamlined nature of the off-line capillary reconditioner offers the advantage of increased system throughput with a minimal increase in system cost.

  16. Validation of capillary blood analysis and capillary testing mode on the epoc Point of Care system

    Directory of Open Access Journals (Sweden)

    Jing Cao

    2017-12-01

    Full Text Available Background: Laboratory test in transport is a critical component of patient care, and capillary blood is a preferred sample type particularly in children. This study evaluated the performance of capillary blood testing on the epoc Point of Care Blood Analysis System (Alere Inc. Methods: Ten fresh venous blood samples was tested on the epoc system under the capillary mode. Correlation with GEM 4000 (Instrumentation Laboratory was examined for Na+, K+, Cl-, Ca2+, glucose, lactate, hematocrit, hemoglobin, pO2, pCO2, and pH, and correlation with serum tested on Vitros 5600 (Ortho Clinical Diagnostics was examined for creatinine. Eight paired capillary and venous blood was tested on epoc and ABL800 (Radiometer for the correlation of Na+, K+, Cl-, Ca2+, glucose, lactate, hematocrit, hemoglobin, pCO2, and pH. Capillary blood from 23 apparently healthy volunteers was tested on the epoc system to assess the concordance to reference ranges used locally. Results: Deming regression correlation coefficients for all the comparisons were above 0.65 except for ionized Ca2+. Accordance of greater than 85% to the local reference ranges were found in all assays with the exception of pO2 and Cl-. Conclusion: Data from this study indicates that capillary blood tests on the epoc system provide comparable results to reference method for these assays, Na+, K+, glucose, lactate, hematocrit, hemoglobin, pCO2, and pH. Further validation in critically ill patients is needed to implement the epoc system in patient transport. Impact of the study: This study demonstrated that capillary blood tests on the epoc Point of Care Blood Analysis System give comparable results to other chemistry analyzers for major blood gas and critical tests. The results are informative to institutions where pre-hospital and inter-hospital laboratory testing on capillary blood is a critical component of patient point of care testing. Keywords: Epoc, Capillary, Transport, Blood gas, Point of care

  17. Demonstration of containment purge and vent valve operability for the Hope Creek Generating Station, Unit 1 (Docket No. 50-354)

    International Nuclear Information System (INIS)

    Kido, C.

    1985-05-01

    The containment purge and vent valve qualification program for the Hope Creek Generating Station has been reviewed by the NRC Licensing Support Section. The review indicates that the licensee has demonstrated the dependability of containment isolation against the buildup of containment pressure due to a LOCA/DBA with the restrictions that during operating conditions 1, 2, and 3 all purge and vent valves will be sealed closed and under administrative control, and during power ascension and descension conditions the 26 in. inboard valve (1-GS-HV-4952) will be used in series with the 2 in. bypass valve (1-GS-HV-4951) to control the release of containment pressure

  18. On Capillary Rise and Nucleation

    Science.gov (United States)

    Prasad, R.

    2008-01-01

    A comparison of capillary rise and nucleation is presented. It is shown that both phenomena result from a balance between two competing energy factors: a volume energy and a surface energy. Such a comparison may help to introduce nucleation with a topic familiar to the students, capillary rise. (Contains 1 table and 3 figures.)

  19. Flow characteristics analysis of purge gas in unitary pebble beds by CFD simulation coupled with DEM geometry model for fusion blanket

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Youhua [University of Science and Technology of China, Hefei, Anhui, 230027 (China); Institute of Plasma Physics, Chinese Academy of Sciences, Hefei, Anhui, 230031 (China); Chen, Lei [Institute of Plasma Physics, Chinese Academy of Sciences, Hefei, Anhui, 230031 (China); Liu, Songlin, E-mail: slliu@ipp.ac.cn [Institute of Plasma Physics, Chinese Academy of Sciences, Hefei, Anhui, 230031 (China); Luo, Guangnan [University of Science and Technology of China, Hefei, Anhui, 230027 (China); Institute of Plasma Physics, Chinese Academy of Sciences, Hefei, Anhui, 230031 (China)

    2017-01-15

    Highlights: • A unitary pebble bed was built to analyze the flow characteristics of purge gas based on DEM-CFD method. • Flow characteristics between particles were clearly displayed. • Porosity distribution, velocity field distribution, pressure field distribution, pressure drop and the wall effects on velocity distribution were studied. - Abstract: Helium is used as the purge gas to sweep tritium out when it flows through the lithium ceramic and beryllium pebble beds in solid breeder blanket for fusion reactor. The flow characteristics of the purge gas will dominate the tritium sweep capability and tritium recovery system design. In this paper, a computational model for the unitary pebble bed was conducted using DEM-CFD method to study the purge gas flow characteristics in the bed, which include porosity distribution between pebbles, velocity field distribution, pressure field distribution, pressure drop as well as the wall effects on velocity distribution. Pebble bed porosity and velocity distribution with great fluctuations were found in the near-wall region and detailed flow characteristics between pebbles were displayed clearly. The results show that the numerical simulation model has an error with about 11% for estimating pressure drop when compared with the Ergun equation.

  20. Validation of capillary blood analysis and capillary testing mode on the epoc Point of Care system.

    Science.gov (United States)

    Cao, Jing; Edwards, Rachel; Chairez, Janette; Devaraj, Sridevi

    2017-12-01

    Laboratory test in transport is a critical component of patient care, and capillary blood is a preferred sample type particularly in children. This study evaluated the performance of capillary blood testing on the epoc Point of Care Blood Analysis System (Alere Inc). Ten fresh venous blood samples was tested on the epoc system under the capillary mode. Correlation with GEM 4000 (Instrumentation Laboratory) was examined for Na+, K+, Cl-, Ca2+, glucose, lactate, hematocrit, hemoglobin, pO2, pCO2, and pH, and correlation with serum tested on Vitros 5600 (Ortho Clinical Diagnostics) was examined for creatinine. Eight paired capillary and venous blood was tested on epoc and ABL800 (Radiometer) for the correlation of Na+, K+, Cl-, Ca2+, glucose, lactate, hematocrit, hemoglobin, pCO2, and pH. Capillary blood from 23 apparently healthy volunteers was tested on the epoc system to assess the concordance to reference ranges used locally. Deming regression correlation coefficients for all the comparisons were above 0.65 except for ionized Ca2+. Accordance of greater than 85% to the local reference ranges were found in all assays with the exception of pO2 and Cl-. Data from this study indicates that capillary blood tests on the epoc system provide comparable results to reference method for these assays, Na+, K+, glucose, lactate, hematocrit, hemoglobin, pCO2, and pH. Further validation in critically ill patients is needed to implement the epoc system in patient transport. This study demonstrated that capillary blood tests on the epoc Point of Care Blood Analysis System give comparable results to other chemistry analyzers for major blood gas and critical tests. The results are informative to institutions where pre-hospital and inter-hospital laboratory testing on capillary blood is a critical component of patient point of care testing.

  1. Separation of isotopes by cyclical processes

    International Nuclear Information System (INIS)

    Hamrin, C.E. Jr.; Weaver, K.

    1976-01-01

    Various isotopes of hydrogen are separated by a cyclic sorption process in which a gas stream containing the isotopes is periodically passed through a high pressure column containing a palladium sorbent. A portion of the product from the high pressure column is passed through a second column at lower pressure to act as a purge. Before the sorbent in the high pressure column becomes saturated, the sequence is reversed with the stream flowing through the former low-pressure column now at high pressure, and a portion of the product purging the former high pressure column now at low pressure. The sequence is continued in cyclic manner with the product being enriched in a particular isotope

  2. Evaluation of highly polar ionic liquid gas chromatographic column for the determination of the fatty acids in milk fat.

    Science.gov (United States)

    Delmonte, Pierluigi; Fardin-Kia, Ali Reza; Kramer, John K G; Mossoba, Magdi M; Sidisky, Len; Tyburczy, Cynthia; Rader, Jeanne I

    2012-04-13

    The SLB-IL111, a new ionic liquid capillary column for gas chromatography available from Supelco Inc., was recently shown to provide enhanced separation of unsaturated geometric and positional isomers of fatty acid (FAs) when it was compared to cyanopropylsiloxane (CPS) columns currently recommended for the analysis of fatty acid methyl esters (FAMEs). A 200 m SLB-IL111 capillary column, operated under a combined temperature and eluent flow gradient, was successfully used to resolve most of the FAs contained in milk fat in a single 80 min chromatographic separation. The selected chromatographic conditions provided a balanced, simultaneous separation of short-chain (from 4:0), long-chain polyunsaturated fatty acids (PUFAs), and most of the unsaturated FA positional/geometric isomers contained in milk fat. Among the monounsaturated fatty acids (MUFAs), these conditions separated t11-18:1 and t10-18:1 FAs, the two most abundant trans fatty acids (t-FA) contained in most dairy products. These t-FAs reportedly have different biological activities. The conjugated linoleic acid (CLA) isomers commonly found in dairy products were separated from each other, including t7,c9-18:2 from c9,t11-18:2, which eliminated the need for their complementary silver ion HPLC analysis. The application of the SLB-IL111 column provided a complementary elution profile of FAMEs to those obtained by CPS columns, allowing for a more comprehensive FA analysis of total milk fat. The FAMEs were identified by the use of available reference materials, previously synthesized and characterized reference mixtures, and prior separations of the milk fat FAMEs by silver ion chromatography based on the number/geometry of double bonds. Published by Elsevier B.V.

  3. Determination of melatonin in wine and plant extracts by capillary electrochromatography with immobilized carboxylic multi-walled carbon nanotubes as stationary phase.

    Science.gov (United States)

    Stege, Patricia W; Sombra, Lorena L; Messina, Germán; Martinez, Luis D; Silva, María F

    2010-07-01

    The finding of melatonin, the often called "hormone of darkness" in plants opens an interesting perspective associated to the plethora of health benefits related to the moderate consumption of red wine. In this study, the implementation of a new method for the determination of melatonin in complex food matrices by CEC with immobilized carboxylic multi-walled carbon nanotubes as stationary phase is demonstrated. The results indicated high electrochromatographic resolution, good capillary efficiencies and improved sensitivity respect to those obtained with conventional capillaries. In addition, it was demonstrated highly reproducible results between runs, days and columns. The LOD for melatonin was 0.01 ng/mL. The method was successfully applied to the determination of melatonin in red and white wine, grape skin and plant extracts of Salvia officinalis L.

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

    Science.gov (United States)

    Schweiger, Susanne; Hinterberger, Stephan; Jungbauer, Alois

    2017-12-08

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

  5. [Determination of penicillin intermediate and three penicillins in milk by high performance capillary electrophoresis].

    Science.gov (United States)

    Tian, Chunqiu; Tan, Huarong; Gao, Liping; Shen, Huqin; Qi, Kezong

    2011-11-01

    A high performance capillary electrophoresis (HPCE) method was developed for the simultaneous determination of penicillin intermediate and penicillins in milk, including 6-amino-penicillanic acid (6-APA), penicillin G (PEN), ampicillin (AMP) and amoxicillin (AMO). The main parameters including the ion concentration and pH value of running buffer, separation voltage and column temperature were optimized systematically by orthogonal test. The four penicillins (PENs) were baseline separated within 4.5 min with the running buffer of 40 mmol/L potassium dihydrogen phosphate-20 mmol/L borax solution (pH 7.8), separation voltage of 28 kV and column temperature of 30 degrees C. The calibration curves showed good linearity in the range of 1.56 - 100 mg/L, and the correlation coefficients (r2) were between 0.9979 and 0.9998. The average recoveries at three spiked levels were in the range of 84.91% - 96.72% with acceptable relative standard deviations (RSDs) of 1.11% - 9.11%. The method is simple, fast, accurate and suitable for the determination of penicillins in real samples.

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

    Science.gov (United States)

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

    2008-01-01

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

  7. Innovative method of direct determination of the content of paraffins, naphthenes, aromatics and sulfur compounds by capillary high-resolution gas chromatography

    Directory of Open Access Journals (Sweden)

    R. Baizhumanova

    2012-03-01

    Full Text Available Based on determination of individual Hydrocarbon (paraffins, naphthenes, aromatics and Sulphur components of fuels and their mixture on the thin bonded of absorber (the stationary phase is a 100-metre silica capillary column, containing 0.5μm film thickness of bonded dimethylpolysiloxane phase by means of the selective solvents (mobile phase combined with technique of ionization of separated compounds by Flame Ionization Detector (FID and Sulphur Chemiluminescence Detector (SCD.

  8. Capillary Pumped Heat Transfer (CHT) Experiment

    Science.gov (United States)

    Hallinan, Kevin P.; Allen, J. S.

    1998-01-01

    The operation of Capillary Pumped Loops (CPL's) in low gravity has generally been unable to match ground-based performance. The reason for this poorer performance has been elusive. In order to investigate the behavior of a CPL in low-gravity, an idealized, glass CPL experiment was constructed. This experiment, known as the Capillary-driven Heat Transfer (CHT) experiment, was flown on board the Space Shuttle Columbia in July 1997 during the Microgravity Science Laboratory mission. During the conduct of the CHT experiment an unexpected failure mode was observed. This failure mode was a result of liquid collecting and then eventually bridging the vapor return line. With the vapor return line blocked, the condensate was unable to return to the evaporator and dry-out subsequently followed. The mechanism for this collection and bridging has been associated with long wavelength instabilities of the liquid film forming in the vapor return line. Analysis has shown that vapor line blockage in present generation CPL devices is inevitable. Additionally, previous low-gravity CPL tests have reported the presence of relatively low frequency pressure oscillations during erratic system performance. Analysis reveals that these pressure oscillations are in part a result of long wavelength instabilities present in the evaporator pores, which likewise lead to liquid bridging and vapor entrapment in the porous media. Subsequent evaporation to the trapped vapor increases the vapor pressure. Eventually the vapor pressure causes ejection of the bridged liquid. Recoil stresses depress the meniscus, the vapor pressure rapidly increases, and the heated surface cools. The process then repeats with regularity.

  9. Transient behavior of a supersonic three-dimensional micronozzle with an intersecting capillary

    Science.gov (United States)

    Matlis, N. H.; Gonsalves, A. J.; Steinke, S.; van Tilborg, J.; Shaw, B.; Mittelberger, D. E.; Geddes, C. G. R.; Leemans, W. P.

    2016-02-01

    An analysis of the interaction between a pulsed, supersonic microjet and an intersecting gas-filled capillary is presented, which enables a direct measurement of the pressure evolution inside the nozzle of the microjet. Plasma-emission spectroscopy was used to resolve, on a sub-microsecond timescale, the build-up and decay of pressure in the nozzle, which are shown to be correlated to the volume of the plenum supplying the nozzle and to the nozzle-throat size, respectively. The microjet, which was integrated with a capillary-discharge waveguide in a sapphire structure, was used to create a small, tunable region of high density gas within a centimeter-scale plateau of lower-density for use in a laser-plasma accelerator. The resultant longitudinally structured gas-density profile has been used to provide control of electron trapping and acceleration, but its evolution has not previously been directly quantified. The results presented here pave the way for improved control of laser-plasma accelerators and are also relevant to applications such as miniature satellites and lab-on-a-chip where precise knowledge of microjet pressure evolution is critical.

  10. Optrode for sensing hydrocarbons

    Science.gov (United States)

    Miller, H.; Milanovich, F.P.; Hirschfeld, T.B.; Miller, F.S.

    1988-09-13

    A two-phase system employing the Fujiwara reaction is provided for the fluorometric detection of halogenated hydrocarbons. A fiber optic is utilized to illuminate a column of pyridine trapped in a capillary tube coaxially attached at one end to the illuminating end of the fiber optic. A strongly alkaline condition necessary for the reaction is maintained by providing a reservoir of alkali in contact with the column of pyridine, the surface of contact being adjacent to the illuminating end of the fiber optic. A semipermeable membrane caps the other end of the capillary tube, the membrane being preferentially permeable to the halogenated hydrocarbon and but preferentially impermeable to water and pyridine. As the halogenated hydrocarbon diffuses through the membrane and into the column of pyridine, fluorescent reaction products are formed. Light propagated by the fiber optic from a light source, excites the fluorescent products. Light from the fluorescence emission is also collected by the same fiber optic and transmitted to a detector. The intensity of the fluorescence gives a measure of the concentration of the halogenated hydrocarbons. 5 figs.

  11. Capillary Interactions between a Probe Tip and a Nanoparticle

    International Nuclear Information System (INIS)

    Li-Ning, Sun; Le-Feng, Wang; Wei-Bin, Rong

    2008-01-01

    To understand capillary interactions between probe tips and nanoparticles under ambient conditions, a theoretical model of capillary forces between them is developed based on the geometric relations. It is found that the contribution of surface tension force to the total capillary force attains to similar order of magnitude as the capillary pressure force in many cases. It is also shown that the tip shape and the radial distance of the meniscus have great influence on the capillary force. The capillary force decreases with the increasing separation distances, and the variance of the contact angles may change the magnitudes of capillary forces several times at large radial distances. The applicability of the symmetric meniscus approximation is discussed. (condensed matter: structure, mechanical and thermal properties)

  12. Comprehensive profiling of ribonucleosides modification by affinity zirconium oxide-silica composite monolithic column online solid-phase microextraction - Mass spectrometry analysis.

    Science.gov (United States)

    Jiang, Han-Peng; Chu, Jie-Mei; Lan, Meng-Dan; Liu, Ping; Yang, Na; Zheng, Fang; Yuan, Bi-Feng; Feng, Yu-Qi

    2016-09-02

    More than 140 modified ribonucleosides have been identified in RNA. Determination of endogenous modified ribonucleosides in biological fluids may serve as non-invasive disease diagnostic strategy. However, detection of the modified ribonucleosides in biological fluids is challenging, especially for the low abundant modified ribonucleosides due to the serious matrix interferences of biological fluids. Here, we developed a facile preparation strategy and successfully synthesized zirconium oxide-silica (ZrO2/SiO2) composite capillary monolithic column that exhibited excellent performance for the selective enrichment of cis-diol-containing compounds. Compared with the boronate-based affinity monolith, the ZrO2/SiO2 monolith showed ∼2 orders of magnitude higher extraction capacity and can be used under physiological pH (pH 6.5-7.5). Using the prepared ZrO2/SiO2 composite monolith as the trapping column and reversed-phase C18 column as the analytical column, we further established an online solid-phase microextraction (SPME) in combination with liquid chromatography-mass spectrometry (online SPME-LC-MS/MS) analysis for the comprehensive profiling of ribonucleosides modification in human urine. Our results showed that 68 cis-diol-containing ribosylated compounds were identified in human urine, which is, to the best of our knowledge, the highest numbers of cis-diol-containing compounds were determined in a single analysis. It is worth noting that four modified ribonucleosides were discovered in the human urine for the first time. In addition, the quantification results from the pooled urine samples showed that compared to healthy controls, the contents of sixteen ribose conjugates in the urine of gastric cancer, eleven in esophagus cancer and seven in lymphoma increased more than two folds. Among these ribose conjugates, four ribose conjugates increased more than two folds in both gastric cancer and esophagus cancer; three ribose conjugates increased more than two

  13. Fast and repetitive in-capillary production of [18F]FDG.

    Science.gov (United States)

    Wester, Hans-Jürgen; Schoultz, Bent Wilhelm; Hultsch, Christina; Henriksen, Gjermund

    2009-04-01

    The increasing demand for radiopharmaceuticals to be provided reproducibly and flexibly with high frequency for clinical application and animal imaging would be better met by improved or even new strategies for automated tracer production. Radiosynthesis in microfluidic systems, i.e. narrow tubing with a diameter of approximately 50-500 microm, holds promise for providing the means for repetitive multidose and multitracer production. In this study, the performance of a conceptually simple microfluidic device integrated into a fully automated synthesis procedure for in-capillary radiosynthesis (ICR) of clinical grade [(18)F]FDG was evaluated. The instrumental set-up consisted of pumps for reagent and solvent delivery into small mixing chambers, micro-fluidic capillaries, in-process radioactivity monitoring, solid-phase extraction and on-column deprotection of the (18)F-labelled intermediate followed by on-line formulation of [(18)F]FDG. In-capillary(18)F-fluorination of 2.1 micromol 1,3,4,6-tetra-O-acetyl-2-O-trifluoromethanesulphonyl-beta-D-mannopyranose (TATM; precursor for [(18)F]FDG) in acetonitrile (MeCN) at a flow rate of 0.3 ml/min within 40 s and subsequent on-line hydrolysis of the intermediate by treatment with 0.3 M NaOH for 1 min at 40 degrees C resulted in a radiochemical yield of 88 +/- 4% within 97%, MeCN <5 microg/ml) and similar absolute yields (approximately 1.4 GBq). The described ICR process is a simple and efficient alternative to classic radiotracer production systems and provides a comparatively cheap instrumental methodology for the repetitive production of [(18)F]FDG with remarkably high efficiency and high yield under fully automated conditions. Although the results concerning the levels of activity need to be confirmed after installation of the equipment in a suitable GMP hot-cell environment, we expect the instrumental design to allow up-scaling without major difficulties or fundamental restrictions. Furthermore, we are convinced that

  14. Modeling and simulation of ammonia removal from purge gases of ammonia plants using a catalytic Pd-Ag membrane reactor

    International Nuclear Information System (INIS)

    Rahimpour, M.R.; Asgari, A.

    2008-01-01

    In this work, the removal of ammonia from synthesis purge gas of an ammonia plant has been investigated. Since the ammonia decomposition is thermodynamically limited, a membrane reactor is used for complete decomposition. A double pipe catalytic membrane reactor is used to remove ammonia from purge gas. The purge gas is flowing in the reaction side and is converted to hydrogen and nitrogen over nickel-alumina catalyst. The hydrogen is transferred through the Pd-Ag membrane of tube side to the shell side. A mathematical model including conservation of mass in the tube and shell side of reactor is proposed. The proposed model was solved numerically and the effects of different parameters on the rector performance were investigated. The effects of pressure, temperature, flow rate (sweep ratio), membrane thickness and reactor diameter have been investigated in the present study. Increasing ammonia conversion was observed by raising the temperature, sweep ratio and reducing membrane thickness. When the pressure increases, the decomposition is gone toward completion but, at low pressure the ammonia conversion in the outset of reactor is higher than other pressures, but complete destruction of the ammonia cannot be achieved. The proposed model can be used for design of an industrial catalytic membrane reactor for removal of ammonia from ammonia plant and reducing NO x emissions

  15. Fast and repetitive in-capillary production of [18F]FDG

    International Nuclear Information System (INIS)

    Wester, Hans-Juergen; Schoultz, Bent Wilhelm; Hultsch, Christina; Henriksen, Gjermund

    2009-01-01

    The increasing demand for radiopharmaceuticals to be provided reproducibly and flexibly with high frequency for clinical application and animal imaging would be better met by improved or even new strategies for automated tracer production. Radiosynthesis in microfluidic systems, i.e. narrow tubing with a diameter of approximately 50-500 μm, holds promise for providing the means for repetitive multidose and multitracer production. In this study, the performance of a conceptually simple microfluidic device integrated into a fully automated synthesis procedure for in-capillary radiosynthesis (ICR) of clinical grade [ 18 F]FDG was evaluated. The instrumental set-up consisted of pumps for reagent and solvent delivery into small mixing chambers, μ-fluidic capillaries, in-process radioactivity monitoring, solid-phase extraction and on-column deprotection of the 18 F-labelled intermediate followed by on-line formulation of [ 18 F]FDG. In-capillary 18 F-fluorination of 2.1 μmol 1,3,4,6-tetra-O-acetyl-2-O-trifluoromethanesulphonyl-beta-d-mannopyranose (TATM; precursor for [ 18 F]FDG) in acetonitrile (MeCN) at a flow rate of 0.3 ml/min within 40 s and subsequent on-line hydrolysis of the intermediate by treatment with 0.3 M NaOH for 1 min at 40 C resulted in a radiochemical yield of 88 ± 4% within 18 F-fluorination was demonstrated by eight independent, sequentially performed ICRs which provided identical tracer quality (radiochemical purity >97%, MeCN 18 F]FDG with remarkably high efficiency and high yield under fully automated conditions. Although the results concerning the levels of activity need to be confirmed after installation of the equipment in a suitable GMP hot-cell environment, we expect the instrumental design to allow up-scaling without major difficulties or fundamental restrictions. Furthermore, we are convinced that similar or nearly identical procedures, and thus instrumentation, will allow ICR of other 18 F-labelled radiopharmaceuticals. (orig.)

  16. Physiological factors influencing capillary growth.

    Science.gov (United States)

    Egginton, S

    2011-07-01

    (1) Angiogenesis (growth of new capillaries from an existing capillary bed) may result from a mismatch in microvascular supply and metabolic demand (metabolic error signal). Krogh examined the distribution and number of capillaries to explore the correlation between O(2) delivery and O(2) consumption. Subsequently, the heterogeneity in angiogenic response within a muscle has been shown to reflect either differences in fibre type composition or mechanical load. However, local control leads to targetted angiogenesis in the vicinity of glycolytic fibre types following muscle stimulation, or oxidative fibres following endurance training, while heterogeneity of capillary spacing is maintained during ontogenetic growth. (2) Despite limited microscopy resolution and lack of specific markers, Krogh's interest in the structure of the capillary wall paved the way for understanding the mechanisms of capillary growth. Angiogenesis may be influenced by the response of perivascular or stromal cells (fibroblasts, macrophages and pericytes) to altered activity, likely acting as a source for chemical signals modulating capillary growth such as vascular endothelial growth factor. In addition, haemodynamic factors such as shear stress and muscle stretch play a significant role in adaptive remodelling of the microcirculation. (3) Most indices of capillarity are highly dependent on fibre size, resulting in possible bias because of scaling. To examine the consequences of capillary distribution, it is therefore helpful to quantify the area of tissue supplied by individual capillaries. This allows the spatial limitations inherent in most models of tissue oxygenation to be overcome generating an alternative approach to Krogh's tissue cylinder, the capillary domain, to improve descriptions of intracellular oxygen diffusion. © 2010 The Author. Acta Physiologica © 2010 Scandinavian Physiological Society.

  17. Separation of oligopeptides, nucleobases, nucleosides and nucleotides using capillary electrophoresis/electrochromatography with sol-gel modified inner capillary wall.

    Science.gov (United States)

    Svobodová, Jana; Kofroňová, Olga; Benada, Oldřich; Král, Vladimír; Mikšík, Ivan

    2017-09-29

    The aim of this article is to study the modification of an inner capillary wall with sol-gel coating (pure silica sol-gel or silica sol-gel containing porphyrin-brucine conjugate) and determine its influence on the separation process using capillary electrophoresis/electrochromatography method. After modification of the inner capillary surface the separation of analytes was performed using two different phosphate buffers (pH 2.5 and 9.0) and finally the changes in electrophoretic mobilities of various samples were calculated. To confirm that the modification of the inner capillary surface was successful, the parts of the inner surfaces of capillaries were observed using scanning electron microscopy. The analytes used as testing samples were oligopeptides, nucleosides, nucleobases and finally nucleotides. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Method of analysis and quality-assurance practices for determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry at the U.S. Geological Survey California District Organic Chemistry Laboratory, 1996-99

    Science.gov (United States)

    Crepeau, Kathryn L.; Baker, Lucian M.; Kuivila, Kathryn

    2000-01-01

    A method of analysis and quality-assurance practices were developed to study the fate and transport of pesticides in the San Francisco Bay-Estuary by the U.S. Geological Survey. Water samples were filtered to remove suspended-particulate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide and the pesticides were eluted with three cartridge volumes of hexane:diethyl ether (1:1) solution. The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for pesticides ranged from 0.002 to 0.025 microgram per liter for 1-liter samples. Recoveries ranged from 44 to 140 percent for 25 pesticides in samples of organic-free reagent water and Sacramento-San Joaquin Delta and Suisun Bay water fortified at 0.05 and 0.50 microgram per liter. The estimated holding time for pesticides after extraction on C-8 solid-phase extraction cartridges ranged from 10 to 257 days.

  19. Improved Peak Capacity for Capillary Electrophoretic Separations of Enzyme Inhibitors with Activity-Based Detection Using Magnetic Bead Microreactors

    Science.gov (United States)

    Yan, Xiaoyan; Gilman, S. Douglass

    2010-01-01

    A technique for separating and detecting enzyme inhibitors was developed using capillary electrophoresis with an enzyme microreactor. The on-column enzyme microreactor was constructed using NdFeB magnet(s) to immobilize alkaline phosphatase-coated superparamagnetic beads (2.8 μm diameter) inside a capillary before the detection window. Enzyme inhibition assays were performed by injecting a plug of inhibitor into a capillary filled with the substrate, AttoPhos. Product generated in the enzyme microreactor was detected by laser-induced fluorescence. Inhibitor zones electrophoresed through the capillary, passed through the enzyme microreactor, and were observed as negative peaks due to decreased product formation. The goal of this study was to improve peak capacities for inhibitor separations relative to previous work, which combined continuous engagement electrophoretically mediated microanalysis (EMMA) and transient engagement EMMA to study enzyme inhibition. The effects of electric field strength, bead injection time and inhibitor concentrations on peak capacity and peak width were investigated. Peak capacities were increased to ≥20 under optimal conditions of electric field strength and bead injection time for inhibition assays with arsenate and theophylline. Five reversible inhibitors of alkaline phosphatase (theophylline, vanadate, arsenate, L-tryptophan and tungstate) were separated and detected to demonstrate the ability of this technique to analyze complex inhibitor mixtures. PMID:20024913

  20. Nanoparticle-based capillary electroseparation of proteins in polymer capillaries under physiological conditions

    DEFF Research Database (Denmark)

    Nilsson, C.; Harwigsson, I.; Becker, K.

    2010-01-01

    Totally porous lipid-based liquid crystalline nanoparticles were used as pseudostationary phase for capillary electroseparation with LIF detection of proteins at physiological conditions using unmodified cyclic olefin copolymer capillaries (Topas (R), 6.7 cm effective length). In the absence of n...... at protein friendly conditions. The developed capillary-based method facilitates future electrochromatography of proteins on polymer-based microchips under physiological conditions and enables the initial optimization of separation conditions in parallel to the chip development....

  1. Western Blotting using Capillary Electrophoresis

    OpenAIRE

    Anderson, Gwendolyn J.; Cipolla, Cynthia; Kennedy, Robert T.

    2011-01-01

    A microscale Western blotting system based on separating sodium-dodecyl sulfate protein complexes by capillary gel electrophoresis followed by deposition onto a blotting membrane for immunoassay is described. In the system, the separation capillary is grounded through a sheath capillary to a mobile X-Y translation stage which moves a blotting membrane past the capillary outlet for protein deposition. The blotting membrane is moistened with a methanol and buffer mixture to facilitate protein a...

  2. Research on the separation properties of empty-column gas chromatography (EC-GC) and conditions for simulated distillation (SIMDIS).

    Science.gov (United States)

    Boczkaj, Grzegorz; Kamiński, Marian

    2013-10-01

    Previous studies have revealed it is possible to separate a high-boiling mixture by gas chromatography in empty fused-silica capillary tubing rather than in columns coated with stationary phase. Chromatographic separation occurs solely on the basis of the different boiling points of the substances separated. The high similarity of such separations to those in classic distillation seems advantageous when gas chromatography is used for simulated distillation. This paper presents results from further research on the separation properties of empty fused silica tubing. The efficiency of this chromatographic system has been examined. The usefulness of such conditions has been studied for simulated distillation, i.e. to determine the boiling-point distribution of complex mixtures, mainly petroleum fractions and products, on the basis of their retention relative to reference substances. The results obtained by use of empty-column gas chromatography (EC-GC) and by use of classical simulated distillation columns have been compared for solutes of different polarity. Studies revealed boiling points determined by EC-GC were more accurate than those obtained by the standard method of simulated distillation.

  3. Simultaneous determination of caffeine, paracetamol, and ibuprofen in pharmaceutical formulations by high-performance liquid chromatography with UV detection and by capillary electrophoresis with conductivity detection.

    Science.gov (United States)

    Cunha, Rafael R; Chaves, Sandro C; Ribeiro, Michelle M A C; Torres, Lívia M F C; Muñoz, Rodrigo A A; Dos Santos, Wallans T P; Richter, Eduardo M

    2015-05-01

    Paracetamol, caffeine and ibuprofen are found in over-the-counter pharmaceutical formulations. In this work, we propose two new methods for simultaneous determination of paracetamol, caffeine and ibuprofen in pharmaceutical formulations. One method is based on high-performance liquid chromatography with diode-array detection and the other on capillary electrophoresis with capacitively coupled contactless conductivity detection. The separation by high-performance liquid chromatography with diode-array detection was achieved on a C18 column (250×4.6 mm(2), 5 μm) with a gradient mobile phase comprising 20-100% acetonitrile in 40 mmol L(-1) phosphate buffer pH 7.0. The separation by capillary electrophoresis with capacitively coupled contactless conductivity detection was achieved on a fused-silica capillary (40 cm length, 50 μm i.d.) using 10 mmol L(-1) 3,4-dimethoxycinnamate and 10 mmol L(-1) β-alanine with pH adjustment to 10.4 with lithium hydroxide as background electrolyte. The determination of all three pharmaceuticals was carried out in 9.6 min by liquid chromatography and in 2.2 min by capillary electrophoresis. Detection limits for caffeine, paracetamol and ibuprofen were 4.4, 0.7, and 3.4 μmol L(-1) by liquid chromatography and 39, 32, and 49 μmol L(-1) by capillary electrophoresis, respectively. Recovery values for spiked samples were between 92-107% for both proposed methods. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Study on the dynamic holdup distribution of the pulsed extraction column

    International Nuclear Information System (INIS)

    Wang, S.; Chen, J.; Wu, Q.

    2013-01-01

    In the study, a CSTR cascade dynamic hydraulic model was developed to investigate the dynamic holdup distribution of the pulsed extraction column. It is assumed that the dynamic process of the dispersed phase holdup of pulsed extraction column has equal effects with the operational process of multiple cascade CSTRs. The process is consistent with the following assumptions: the holdups vary on different stages but maintain uniform on each stage; the changes of the hydraulic parameters have impact initially on the inlet of dispersed phase, and stability will be reached gradually through stage-by-stage blending. The model was tested and verified utilizing time domain response curves of the average holdup. Nearly 150 experiments were carried out with different capillary columns, various feed liquids, and diverse continuous phases and under different operation conditions. The regression curves developed by the model show a good consistency with the experimental results. After linking parameters of the model with operational conditions, the study further found that the parameters are only linearly correlated with pulse conditions and have nothing to do with flow rate for a specific pulsed extraction column. The accuracy of the model is measured by the average holdup, and the absolute error is ±0.01. The model can provide supports for the boundary studies on hydraulics and mass transfer by making simple and reliable prediction of the dynamic holdup distribution, with relatively less accessible hydraulic experimental data. (authors)

  5. Study on the dynamic holdup distribution of the pulsed extraction column

    Energy Technology Data Exchange (ETDEWEB)

    Wang, S.; Chen, J.; Wu, Q. [Tsinghua University, Beijing 100084 (China)

    2013-07-01

    In the study, a CSTR cascade dynamic hydraulic model was developed to investigate the dynamic holdup distribution of the pulsed extraction column. It is assumed that the dynamic process of the dispersed phase holdup of pulsed extraction column has equal effects with the operational process of multiple cascade CSTRs. The process is consistent with the following assumptions: the holdups vary on different stages but maintain uniform on each stage; the changes of the hydraulic parameters have impact initially on the inlet of dispersed phase, and stability will be reached gradually through stage-by-stage blending. The model was tested and verified utilizing time domain response curves of the average holdup. Nearly 150 experiments were carried out with different capillary columns, various feed liquids, and diverse continuous phases and under different operation conditions. The regression curves developed by the model show a good consistency with the experimental results. After linking parameters of the model with operational conditions, the study further found that the parameters are only linearly correlated with pulse conditions and have nothing to do with flow rate for a specific pulsed extraction column. The accuracy of the model is measured by the average holdup, and the absolute error is ±0.01. The model can provide supports for the boundary studies on hydraulics and mass transfer by making simple and reliable prediction of the dynamic holdup distribution, with relatively less accessible hydraulic experimental data. (authors)

  6. Relating pressure tuned coupled column ensembles with the solvation parameter model for tunable selectivity in gas chromatography.

    Science.gov (United States)

    Sharif, Khan M; Kulsing, Chadin; Chin, Sung-Tong; Marriott, Philip J

    2016-07-15

    The differential pressure drop of carrier gas by tuning the junction point pressure of a coupled column gas chromatographic system leads to a unique selectivity of the overall separation, which can be tested using a mixture of compounds with a wide range of polarity. This study demonstrates a pressure tuning (PT) GC system employing a microfluidic Deans switch located at the mid-point of the two capillary columns. This PT system allowed variations of inlet-outlet pressure differences of the two columns in a range of 52-17psi for the upstream column and 31-11psi for the downstream column. Peak shifting (differential migration) of compounds due to PT difference are related to a first order regression equation in a Plackett-Burman factorial study. Increased first (upstream) column pressure drop makes the second column characteristics more significant in the coupled column retention behavior, and conversely increased second (downstream) column pressure drop makes the first column characteristics more apparent; such variation can result in component swapping between polar and non-polar compounds. The coupled column system selectivity was evaluated in terms of linear solvation energy relationship (LSER) parameters, and their relation with different pressure drop effects has been constructed by applying multivariate principle component analysis (PCA). It has been found that the coupled column PT system descriptors provide a result that shows a clear clustering of different pressure settings, somewhat intermediate between those of the two commercial columns. This is equivalent to that obtained from a conventional single-column GC analysis where the interaction energy contributed from the stationary phases can be significantly adjusted by choice of midpoint PT. This result provides a foundation for pressure differentiation for selectivity enhancement. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Multivariate optimization of headspace trap for furan and furfural simultaneous determination in sponge cake.

    Science.gov (United States)

    Cepeda-Vázquez, Mayela; Blumenthal, David; Camel, Valérie; Rega, Barbara

    2017-03-01

    Furan, a possibly carcinogenic compound to humans, and furfural, a naturally occurring volatile contributing to aroma, can be both found in thermally treated foods. These process-induced compounds, formed by close reaction pathways, play an important role as markers of food safety and quality. A method capable of simultaneously quantifying both molecules is thus highly relevant for developing mitigation strategies and preserving the sensory properties of food at the same time. We have developed a unique reliable and sensitive headspace trap (HS trap) extraction method coupled to GC-MS for the simultaneous quantification of furan and furfural in a solid processed food (sponge cake). HS Trap extraction has been optimized using an optimal design of experiments (O-DOE) approach, considering four instrumental and two sample preparation variables, as well as a blocking factor identified during preliminary assays. Multicriteria and multiple response optimization was performed based on a desirability function, yielding the following conditions: thermostatting temperature, 65°C; thermostatting time, 15min; number of pressurization cycles, 4; dry purge time, 0.9min; water / sample amount ratio (dry basis), 16; and total amount (water + sample amount, dry basis), 10g. The performances of the optimized method were also assessed: repeatability (RSD: ≤3.3% for furan and ≤2.6% for furfural), intermediate precision (RSD: 4.0% for furan and 4.3% for furfural), linearity (R 2 : 0.9957 for furan and 0.9996 for furfural), LOD (0.50ng furan g sample dry basis -1 and 10.2ng furfural g sample dry basis -1 ), LOQ (0.99ng furan g sample dry basis -1 and 41.1ng furfural g sample dry basis -1 ). Matrix effect was observed mainly for furan. Finally, the optimized method was applied to other sponge cakes with different matrix characteristics and levels of analytes. Copyright © 2016. Published by Elsevier B.V.

  8. Indirect fluorescence detection of native amino acids in capillary zone electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Kuhr, W.G.; Yeung, E.S.

    1988-09-01

    Amino acids are but one of several important classes of small chemical compounds in biological chemistry that have an inherent lack of analytically useful physical properties. Amino acids, peptides, fatty acids, sugars, many mono-, di-, and tricarboxylic acids, and phosphorylated intermediates in glycolysis and metabolism show little, if any, UV or visible absorption, fluorescence, or electrochemical activity. As the emphasis of biochemical research shifts to smaller samples where, for example, picomolar quantities of amino acids are analyzed in gas phase protein sequencing or in microliter samples of the extracellular fluid of the mammalian brain, the analytical problem becomes even more challenging due to the small volume of sample available for analysis. In this work, laser-induced fluorescence spectroscopy is performed on-column to detect the bands separated with capillary zone electrophoresis (CZE). CZE is an instrumental form of zone electrophoresis where chemical species are separated purely on the basis of their electrophoretic mobility, since no supporting gel is utilized. Both anions and cations can be separated in the same run because of the large electroosmotic flow generated in small diameter capillaries. This technique has already been used successfully in the rapid, efficient separation of dansyl-amino acids.

  9. Reciprocal associations between negative affect, binge eating, and purging in the natural environment in women with bulimia nervosa.

    Science.gov (United States)

    Lavender, Jason M; Utzinger, Linsey M; Cao, Li; Wonderlich, Stephen A; Engel, Scott G; Mitchell, James E; Crosby, Ross D

    2016-04-01

    Although negative affect (NA) has been identified as a common trigger for bulimic behaviors, findings regarding NA following such behaviors have been mixed. This study examined reciprocal associations between NA and bulimic behaviors using real-time, naturalistic data. Participants were 133 women with bulimia nervosa (BN) according to the 4th edition of the Diagnostic and Statistical Manual of Mental Disorders who completed a 2-week ecological momentary assessment protocol in which they recorded bulimic behaviors and provided multiple daily ratings of NA. A multilevel autoregressive cross-lagged analysis was conducted to examine concurrent, first-order autoregressive, and prospective associations between NA, binge eating, and purging across the day. Results revealed positive concurrent associations between all variables across all time points, as well as numerous autoregressive associations. For prospective associations, higher NA predicted subsequent bulimic symptoms at multiple time points; conversely, binge eating predicted lower NA at multiple time points, and purging predicted higher NA at 1 time point. Several autoregressive and prospective associations were also found between binge eating and purging. This study used a novel approach to examine NA in relation to bulimic symptoms, contributing to the existing literature by directly examining the magnitude of the associations, examining differences in the associations across the day, and controlling for other associations in testing each effect in the model. These findings may have relevance for understanding the etiology and/or maintenance of bulimic symptoms, as well as potentially informing psychological interventions for BN. (c) 2016 APA, all rights reserved).

  10. Ion Chromatographic Analyses of Sea Waters, Brines and Related Samples

    Directory of Open Access Journals (Sweden)

    Nataša Gros

    2013-06-01

    Full Text Available This review focuses on the ion chromatographic methods for the analyses of natural waters with high ionic strength. At the beginning a natural diversity in ionic composition of waters is highlighted and terminology clarified. In continuation a brief overview of other review articles of potential interest is given. A review of ion chromatographic methods is organized in four sections. The first section comprises articles focused on the determination of ionic composition of water samples as completely as possible. The sections—Selected Anions, Selected Cations and Metals—follow. The most essential experimental conditions used in different methods are summarized in tables for a rapid comparison. Techniques encountered in the reviewed articles comprise: direct determinations of ions in untreated samples with ion- or ion-exclusion chromatography, or electrostatic ion chromatography; matrix elimination with column-switching; pre-concentration with a chelation ion chromatography and purge-and-trap pre-concentration. Different detection methods were used: non-suppressed conductometric or suppressed conductometric, direct spectrometric or spectrometric after a post-column derivetization, and inductively coupled plasma in combination with optical emission or mass spectrometry.

  11. Measurement of Capillary Radius and Contact Angle within Porous Media.

    Science.gov (United States)

    Ravi, Saitej; Dharmarajan, Ramanathan; Moghaddam, Saeed

    2015-12-01

    The pore radius (i.e., capillary radius) and contact angle determine the capillary pressure generated in a porous medium. The most common method to determine these two parameters is through measurement of the capillary pressure generated by a reference liquid (i.e., a liquid with near-zero contact angle) and a test liquid. The rate of rise technique, commonly used to determine the capillary pressure, results in significant uncertainties. In this study, we utilize a recently developed technique for independently measuring the capillary pressure and permeability to determine the equivalent minimum capillary radii and contact angle of water within micropillar wick structures. In this method, the experimentally measured dryout threshold of a wick structure at different wicking lengths is fit to Darcy's law to extract the maximum capillary pressure generated by the test liquid. The equivalent minimum capillary radii of different wick geometries are determined by measuring the maximum capillary pressures generated using n-hexane as the working fluid. It is found that the equivalent minimum capillary radius is dependent on the diameter of pillars and the spacing between pillars. The equivalent capillary radii of micropillar wicks determined using the new method are found to be up to 7 times greater than the current geometry-based first-order estimates. The contact angle subtended by water at the walls of the micropillars is determined by measuring the capillary pressure generated by water within the arrays and the measured capillary radii for the different geometries. This mean contact angle of water is determined to be 54.7°.

  12. An efficient hydrophilic interaction liquid chromatography separation of 7 phospholipid classes based on a diol column

    NARCIS (Netherlands)

    Zhu, C.; Dane, A.; Spijksma, G.; Wang, M.; Greef, J. van der; Luo, G.; Hankemeier, T.; Vreeken, R.J.

    2012-01-01

    A hydrophilic interaction liquid chromatography (HILIC) - ion trap mass spectrometry method was developed for separation of a wide range of phospholipids. A diol column which is often used with normal phase chromatography was adapted to separate different phospholipid classes in HILIC mode using a

  13. Equations for nickel-chromium wire heaters of column transfer lines in gas chromatographic-electroantennographic detection (GC-EAD).

    Science.gov (United States)

    Byers, John A

    2004-05-30

    Heating of chromatographic columns, transfer lines, and other devices is often required in neuroscience research. For example, volatile compounds passing through a capillary column of a gas chromatograph (GC) can be split, with half exiting the instrument through a heated transfer line to an insect antenna or olfactory sensillum for electroantennographic detector (GC-EAD) recordings. The heated transfer line is used to prevent condensation of various chemicals in the capillary that would otherwise occur at room temperature. Construction of such a transfer line heater is described using (80/20%) nickel-chromium heating wire wrapped in a helical coil and powered by a 120/220 V ac rheostat. Algorithms were developed in a computer program to estimate the voltage at which a rheostat should be set to obtain the desired heater temperature for a specific coil. The coil attributes (radius, width, number of loops, or length of each loop) are input by the user, as well as AWG size of heating wire and desired heater temperature. The program calculates total length of wire in the helix, resistance of the wire, amperage used, and the voltage to set the rheostat. A discussion of semiochemical isolation methods using the GC-EAD and bioassays is presented.

  14. Capillary Thinning and Pinch-off Dynamics and Printability of Polyelectrolyte Solutions

    Science.gov (United States)

    Sharma, Vivek; Jimenez, Leidy N.; Dinic, Jelena; Parsi, Nikila

    Biological macromolecules like proteins, DNA and polysaccharides, and many industrial polymers, are classified together as polyelectrolytes for in solution, the repeat units in their backbone are decorated with disassociated, charge-bearing ionic groups, surrounded by counter-ions. In diverse applications like inkjet printing, sprayable cosmetics and insecticides, paints and coatings that involve formation of fluid columns or sheets that undergo progressive thinning and pinch-off into drops, the dominant flow within the necking filament is extensional in nature. The extensional rheology response of the charged macromolecular solutions is not as well understood as that of their uncharged counterparts. Here focus on the characterization of capillary thinning and pinch-off dynamics, extensional rheology and printability of two model systems: sodium (polystyrene sulfonate) and poly(acrylic acid) by using dripping-onto-substrate (DoS) rheometry technique. Both the measured extensional relaxation times and the extensional viscosity values show salt- and polymer concentration-dependent behavior that is not expected or anticipated from the typical shear rheology response.

  15. Modifications of the Cornell University TRIGA reactor thermal column

    International Nuclear Information System (INIS)

    Aderhold, Howard C.

    1984-01-01

    Full text: The thermal column has been modified to provide a horizontal beam suitable for neutron radiography. A hole of circular cross-section was cut along the axis of the thermal column through graphite and lead from the outer surface of the 'sliding block' to a point about 10 cm short of the curved end of the thermal column. The section through the sliding block is 15.2 cm in diameter and the remaining section is 10.2 cm in diameter. The outer or 15.2-cm section is lined with a 6-mm thick Boral sleeve, and the inner or 10.2-cm section contains a tapered collimator of Pd-Cd alloy inside a 3-mm thick Boral sleeve, a defining aperture formed by a 2.5-cm diameter hole in a 6-mm Boral plate, and, at the core end, a 5.1-cm thick bismuth absorber disk. All of these components are enclosed in an aluminum housing. From the sliding block outwards - a distance of 122 cm across the hohlraum and through the graphite at the exit end, plus another 122 cm through the rolling door - no drilling was necessary since removable plugs could be taken out to form a tapered hole of square cross section with stepped widths of 30.5, 33.0, and 38.1 cm. An aluminum housing fitting snugly in this hole is lined with Boral or a gadolinium-bearing paint and is joined with a rubber gasket to the inner housing, so that the entire length can be purged with helium. This system provides an l/d ratio of 1/140 and a useful beam area at the exposure point of 38 cm x 38 cm. At 480 kW, the neutron flux there is 10 6 n/cm 2 sec and the gamma flux is 17 R/hr. Figure 2 is a reproduction of the first radiograph taken with the facility. (author)

  16. Impaired skin capillary recruitment in essential hypertension is caused by both functional and structural capillary rarefaction

    NARCIS (Netherlands)

    Serne, EH; Gans, ROB; ter Maaten, JC; Tangelder, GJ; Donker, AJM; Stehouwer, CDA

    Capillary rarefaction occurs in many tissues in patients with essential hypertension and may contribute to an increased vascular resistance and impaired muscle metabolism. Rarefaction may be caused by a structural (anatomic) absence of capillaries, functional nonperfusion, or both. The aim of this

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

    Science.gov (United States)

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

    2017-08-01

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

  18. Molecularly Imprinted Porous Monolithic Materials from Melamine-Formaldehyde for Selective Trapping of Phosphopeptides

    DEFF Research Database (Denmark)

    Liu, Mingquan; Tran, Tri Minh; Abbas Elhaj, Ahmed Awad

    2017-01-01

    monoliths, chosen based on the combination of meso- and macropores providing optimal percolative flow and accessible surface area, was synthesized in the presence of N-Fmoc and O-Et protected phosphoserine and phosphotyrosine to prepare molecularly imprinted monoliths with surface layers selective...... for phosphopeptides. These imprinted monoliths were characterized alongside nonimprinted monoliths by a variety of techniques and finally evaluated by liquid chromatography-mass spectrometry in the capillary format to assess their abilities to trap and release phosphorylated amino acids and peptides from partly...

  19. Biomedical applications of capillary electrophoresis

    International Nuclear Information System (INIS)

    Kartsova, L A; Bessonova, E A

    2015-01-01

    The review deals with modern analytical approaches used in capillary electrophoresis for solving medical and biological problems: search for biomarkers of various diseases and rapid diagnosis based on characteristic profiles of biologically active compounds by capillary electrophoresis with mass spectrometric detection; monitoring of the residual drugs in biological fluids for evaluating the efficiency of drug therapy; testing of the enantiomeric purity of pharmaceutical products; the use of novel materials as components of stationary and pseudo-stationary phases in capillary electrophoresis and capillary electrochromatography to increase the selectivity of separation of components of complex matrices; and identification of various on-line preconcentration techniques to reduce the detection limits of biologically active analytes. A topical trend in capillary electrophoresis required in clinical practice, viz., the design of microfluidic systems, is discussed. The bibliography includes 173 references

  20. Water-column mass losses during the emptying of a large-scale pipeline by pressurized air

    NARCIS (Netherlands)

    Laanearu, J.; Hou, Q.; Annus, I.; Tijsseling, A.S.

    2015-01-01

    In many industrial applications the liquid trapped inside long pipelines can cause a number of problems. Intrusion of the pressurized air on top of the water column inside the horizontal pipeline can result in a less or more mixed stratified flow. The dynamics of a moving air–water front during the

  1. Monolithic columns based on a poly(styrene-divinylbenzene-methacrylic acid) copolymer for capillary liquid chromatography of small organic molecules

    Czech Academy of Sciences Publication Activity Database

    Svobodová, A.; Křížek, T.; Širc, Jakub; Šálek, Petr; Tesařová, E.; Coufal, P.; Štulík, K.

    2011-01-01

    Roč. 1218, č. 11 (2011), s. 1544-1547 ISSN 0021-9673 R&D Projects: GA AV ČR KAN200520804 Institutional research plan: CEZ:AV0Z40500505 Keywords : capillary liquid chromatography * methacrylic acid * polystyrene-based monolithic stationary phase Subject RIV: EI - Biotechnology ; Bionics Impact factor: 4.531, year: 2011

  2. Analysis of microdialysate monoamines, including noradrenaline, dopamine and serotonin, using capillary ultra-high performance liquid chromatography and electrochemical detection.

    Science.gov (United States)

    Ferry, Barbara; Gifu, Elena-Patricia; Sandu, Ioana; Denoroy, Luc; Parrot, Sandrine

    2014-03-01

    Electrochemical methods are very often used to detect catecholamine and indolamine neurotransmitters separated by conventional reverse-phase high performance liquid chromatography (HPLC). The present paper presents the development of a chromatographic method to detect monoamines present in low-volume brain dialysis samples using a capillary column filled with sub-2μm particles. Several parameters (repeatability, linearity, accuracy, limit of detection) for this new ultrahigh performance liquid chromatography (UHPLC) method with electrochemical detection were examined after optimization of the analytical conditions. Noradrenaline, adrenaline, serotonin, dopamine and its metabolite 3-methoxytyramine were separated in 1μL of injected sample volume; they were detected above concentrations of 0.5-1nmol/L, with 2.1-9.5% accuracy and intra-assay repeatability equal to or less than 6%. The final method was applied to very low volume dialysates from rat brain containing monoamine traces. The study demonstrates that capillary UHPLC with electrochemical detection is suitable for monitoring dialysate monoamines collected at high sampling rate. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Microfluidic Trap Arrays: Passive Sensors for Studying Aquatic Protozoan Ecology and Biogeography

    Science.gov (United States)

    Chau, J. F.; Bouchillon, G.; Shor, L. M.

    2012-12-01

    Microscopic organisms such as bacteria and protozoa are the engine that drives global biogeochemical processes: microbes fix carbon, produce oxygen, mediate nutrient cycling, and break down anthropogenic contaminants. In many habitats, the bacterial community structure and its net production is controlled in a top-down fashion by predation by protozoa. Despite their importance, many researchers have noted a significant gap in our understanding of their diversity, biogeography, and ecosystem function. We developed a microfluidic field sampling and analysis tool to study the biogeography and function of microbial eukaryotes. Microfluidic samplers were created to systematically target the morphology, function, and habitat of different microbial eukaryotes. Features such as channel dimensions, branching angles and radii of curvature were varied to allow organisms to be selected and captured based on cell size, shape, plasticity, and swimming or crawling modalities. We also developed genetic analysis protocols to extract and amplify DNA from a single trapped cell, allowing for molecular identification of trapped species. Results from freshwater sediment and water column deployments confirmed design efficiencies in trapping and concentrating protozoa based on biomass density, allowed for analysis of body plasticity and cell size, and also confirmed the viability of this technology for future real time monitoring of protozoa in aquatic ecosystems. This research offers a radical departure from existing approaches to study microbial eukaryotic communities in the field. Our novel methodology involving trapping, observation and recording of physical characteristics and genetic analysis of single cells allows comparison with bulk samples to place trapped microbes within a function- and habitat-specific context.

  4. Capillary concentrators for synchrotron radiation beamlines

    International Nuclear Information System (INIS)

    Heald, S.M.; Brewe, D.L.; Kim, K.H.; Brown, F.C.; Barg, B.; Stern, E.A.

    1996-01-01

    Capillary concentrators condense x-rays by multiple reflections down a gradually tapering capillary. They can provide sub-micron beam spots, and are promising candidates for use in the next generation x-ray microprobe beamlines. The weak energy dependence of their properties make them especially useful for energy scanning applications such as micro-XAFS. This paper examines the potential performance of capillary optics for an x-ray microprobe, as well as some practical issues such as fabrication and alignment. Best performance at third generation sources requires long capillaries, and the authors have been using fiber optics techniques to fabricate capillaries up to one meter in length. The performance of shorter (less than about 0.5 m) capillaries has often been found to agree well with theoretical calculations, indicating the inner surface is a high quality x-ray reflector. These capillaries have been tested at the NSLS for imaging and micro-XAFS down to 2.6 microm resolution with excellent results. On an unfocused bend magnet line flux density approaching 10 6 ph/sec/microm 2 has been achieved. While nearly optimum profiles have been achieved for longer capillaries, the results have been disappointing, and alignment problems are suspected. The dramatic improvement in performance possible at third generation synchrotrons such as the APS is discussed along with improvements possible by using the capillaries in conjunction with coupling optics

  5. Paul trap experiment to simulate intense nonneutral beam propagation through a periodic focusing field configuration

    CERN Document Server

    Davidson, R C; Majeski, R; Qin, H; Shvets, G

    2001-01-01

    This paper describes the design concept for a compact Paul trap experimental configuration that fully simulates the collective processes and nonlinear transverse dynamics of an intense charged particle beam that propagates over large distances through a periodic quadrupole magnetic field. To summarize, a long nonneutral plasma column (L>=r sub p) is confined axially by applied DC voltages V[circ]=const. on end cylinders at z=+-L, and transverse confinement is provided by segmented cylindrical electrodes (at radius r sub w) with applied oscillatory voltages +-V sub 0 (t) over 90 deg. segments. Because the transverse focusing force is similar in waveform to that produced by a discrete set of periodic quadrupole magnets in a frame moving with the beam, the Paul trap configuration offers the possibility of simulating intense beam propagation in a compact experimental facility. The nominal operating parameters in the experimental design are: barium ions (A=137); plasma column length 2L=2 m; wall radius r sub w =10...

  6. Experimental investigation of virus and clay particles cotransport in partially saturated columns packed with glass beads.

    Science.gov (United States)

    Syngouna, Vasiliki I; Chrysikopoulos, Constantinos V

    2015-02-15

    Suspended clay particles in groundwater can play a significant role as carriers of viruses, because, depending on the physicochemical conditions, clay particles may facilitate or hinder the mobility of viruses. This experimental study examines the effects of clay colloids on the transport of viruses in variably saturated porous media. All cotransport experiments were conducted in both saturated and partially saturated columns packed with glass beads, using bacteriophages MS2 and ΦX174 as model viruses, and kaolinite (KGa-1b) and montmorillonite (STx-1b) as model clay colloids. The various experimental collision efficiencies were determined using the classical colloid filtration theory. The experimental data indicated that the mass recovery of viruses and clay colloids decreased as the water saturation decreased. Temporal moments of the various breakthrough concentrations collected, suggested that the presence of clays significantly influenced virus transport and irreversible deposition onto glass beads. The mass recovery of both viruses, based on total effluent virus concentrations, was shown to reduce in the presence of suspended clay particles. Furthermore, the transport of suspended virus and clay-virus particles was retarded, compared to the conservative tracer. Under unsaturated conditions both clay particles facilitated the transport of ΦX174, while hindered the transport of MS2. Moreover, the surface properties of viruses, clays and glass beads were employed for the construction of classical DLVO and capillary potential energy profiles, and the results suggested that capillary forces play a significant role on colloid retention. It was estimated that the capillary potential energy of MS2 is lower than that of ΦX174, and the capillary potential energy of KGa-1b is lower than that of STx-1b, assuming that the protrusion distance through the water film is the same for each pair of particles. Moreover, the capillary potential energy is several orders of

  7. Role of mixed boundaries on flow in open capillary channels with curved air-water interfaces.

    Science.gov (United States)

    Zheng, Wenjuan; Wang, Lian-Ping; Or, Dani; Lazouskaya, Volha; Jin, Yan

    2012-09-04

    Flow in unsaturated porous media or in engineered microfluidic systems is dominated by capillary and viscous forces. Consequently, flow regimes may differ markedly from conventional flows, reflecting strong interfacial influences on small bodies of flowing liquids. In this work, we visualized liquid transport patterns in open capillary channels with a range of opening sizes from 0.6 to 5.0 mm using laser scanning confocal microscopy combined with fluorescent latex particles (1.0 μm) as tracers at a mean velocity of ∼0.50 mm s(-1). The observed velocity profiles indicate limited mobility at the air-water interface. The application of the Stokes equation with mixed boundary conditions (i.e., no slip on the channel walls and partial slip or shear stress at the air-water interface) clearly illustrates the increasing importance of interfacial shear stress with decreasing channel size. Interfacial shear stress emerges from the velocity gradient from the adjoining no-slip walls to the center where flow is trapped in a region in which capillary forces dominate. In addition, the increased contribution of capillary forces (relative to viscous forces) to flow on the microscale leads to increased interfacial curvature, which, together with interfacial shear stress, affects the velocity distribution and flow pattern (e.g., reverse flow in the contact line region). We found that partial slip, rather than the commonly used stress-free condition, provided a more accurate description of the boundary condition at the confined air-water interface, reflecting the key role that surface/interface effects play in controlling flow behavior on the nanoscale and microscale.

  8. Reactor containment purge and vent valve performance experiments

    International Nuclear Information System (INIS)

    Hunter, J.A.; Steele, R.; Watkins, J.C.

    1985-01-01

    Three nuclear-designed butterfly valves typical of those used in domestic nuclear power plant containment purge and vent applications were tested. For a comparison of responses, two eight-inch nominal pipe size valves with differing internal design were tested. For extrapolation insights, a 24-inch nominal pipe size valve was also tested. The valve experiments were performed with various piping configurations and valve disc orientations to the flow, to simulate various installation options in field application. As a standard for comparing the effects of the installation options, testing was also performed in a standard ANSI test section. Test cycles were performed at inlet pressures of 5 to 60 psig, while monitoring numerous test parameters, such as the valve disc position, valve shaft torque, mass flow rate, and the pressure and temperature at multiple locations throughout the test section. An experimental data base was developed to assist in the evaluation of the current analytical methods and to determine the influence of inlet pressure, inlet duct geometry, and valve orientation to the flow media on valve torque requirements, along with any resulting limitations to the extrapolation methods. 2 refs., 15 figs

  9. Conventional and narrow bore short capillary columns with cyclodextrin derivatives as chiral selectors to speed-up enantioselective gas chromatography and enantioselective gas chromatography-mass spectrometry analyses.

    Science.gov (United States)

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

    2008-11-28

    The analysis of complex real-world samples of vegetable origin requires rapid and accurate routine methods, enabling laboratories to increase sample throughput and productivity while reducing analysis costs. This study examines shortening enantioselective-GC (ES-GC) analysis time following the approaches used in fast GC. ES-GC separations are due to a weak enantiomer-CD host-guest interaction and the separation is thermodynamically driven and strongly influenced by temperature. As a consequence, fast temperature rates can interfere with enantiomeric discrimination; thus the use of short and/or narrow bore columns is a possible approach to speeding-up ES-GC analyses. The performance of ES-GC with a conventional inner diameter (I.D.) column (25 m length x 0.25 mm I.D., 0.15 microm and 0.25 microm d(f)) coated with 30% of 2,3-di-O-ethyl-6-O-tert-butyldimethylsilyl-beta-cyclodextrin in PS-086 is compared to those of conventional I.D. short column (5m length x 0.25 mm I.D., 0.15 microm d(f)) and of different length narrow bore columns (1, 2, 5 and 10 m long x 0.10 mm I.D., 0.10 microm d(f)) in analysing racemate standards of pesticides and in the flavour and fragrance field and real-world-samples. Short conventional I.D. columns gave shorter analysis time and comparable or lower resolutions with the racemate standards, depending mainly on analyte volatility. Narrow-bore columns were tested under different analysis conditions; they provided shorter analysis time and resolutions comparable to those of conventional I.D. ES columns. The narrow-bore columns offering the most effective compromise between separation efficiency and analysis time are the 5 and 2m columns; in combination with mass spectrometry as detector, applied to lavender and bergamot essential oil analyses, these reduced analysis time by a factor of at least three while separation of chiral markers remained unaltered.

  10. Purging of acute myeloid leukaemia cells from stem cell grafts by hyperthermia : enhancement of the therapeutic index by the tetrapeptide AcSDKP and the alkyl-lysophospholipid ET-18-OCH3

    NARCIS (Netherlands)

    Wierenga, PK; Setroikromo, R; Vellenga, E; Kampinga, HH

    2000-01-01

    Hyperthermia has been shown to be a potential purging modality in autologous stem cell transplantation settings owing to its selective toxicity towards leukaemic cells, We describe two approaches to further increase the therapeutic index of the hyperthermic purging modality by using normal murine

  11. [Preparation and performance characterization of gold nanoparticles modified chiral capillary electrochromatography stationary phase].

    Science.gov (United States)

    Xiong, Lele; Li, Ruijun; Ji, Yibing

    2017-07-08

    Gold nanoparticles (GNPs, 15 nm) were prepared and introduced to amino groups derived silica monolithic column. Bovine serum albumin (BSA) was immobilized via covalent modification method onto the carboxylic functionalized GNPs to afford chiral stationary phase (CSP) for enantioseparation. GNPs were well dispersed and successfully incorporated onto the columns with the contents as high as 17.18% by characterization method such as transmission electron microscopy (TEM), ultraviolet (UV)-visible absorption spectra and scanning electron microscopy (SEM). The preparation conditions of the BSA modified CSP were optimized and 10% (v/v) 3-aminopropyltriethoxysilane (APTES) and 15 g/L BSA were selected as appropriate reaction conditions. The enantioseparation performance of the BSA modified CSP has been investigated by capillary electrochromatography (CEC). Enantiomers of tryptophan, ephedrine and atenolol were resolved, and the baseline separation of tryptophan was achieved. Meanwhile, the influences of pH value, buffer concentrations and applied voltages used on the chiral separation were studied, and the optimal separation conditions were 10 mmol/L phosphate buffer at pH 7.4 and 15 kV applied voltages. In comparison with the BSA modified CSP prepared by physical adsorption, the CSP prepared by covalent modification method had better separation results, and the analytes could be separated directly without pre-column derivatization. In addition, the prepared BSA modified CSP exhibited good run to run repeatability with relative standard deviations (RSDs) of the migration times and selectivity factors not more than 2.3% and 0.96%, respectively. This work offers a good thinking for modification with other proteins or other types of chiral selectors.

  12. Capillary pumped loop body heat exchanger

    Science.gov (United States)

    Swanson, Theodore D. (Inventor); Wren, deceased, Paul (Inventor)

    1998-01-01

    A capillary pumped loop for transferring heat from one body part to another body part, the capillary pumped loop comprising a capillary evaporator for vaporizing a liquid refrigerant by absorbing heat from a warm body part, a condenser for turning a vaporized refrigerant into a liquid by transferring heat from the vaporized liquid to a cool body part, a first tube section connecting an output port of the capillary evaporator to an input of the condenser, and a second tube section connecting an output of the condenser to an input port of the capillary evaporator. A wick may be provided within the condenser. A pump may be provided between the second tube section and the input port of the capillary evaporator. Additionally, an esternal heat source or heat sink may be utilized.

  13. Effects of oxide traps, interface traps, and ''border traps'' on metal-oxide-semiconductor devices

    International Nuclear Information System (INIS)

    Fleetwood, D.M.; Winokur, P.S.; Reber, R.A. Jr.; Meisenheimer, T.L.; Schwank, J.R.; Shaneyfelt, M.R.; Riewe, L.C.

    1993-01-01

    We have identified several features of the 1/f noise and radiation response of metal-oxide-semiconductor (MOS) devices that are difficult to explain with standard defect models. To address this issue, and in response to ambiguities in the literature, we have developed a revised nomenclature for defects in MOS devices that clearly distinguishes the language used to describe the physical location of defects from that used to describe their electrical response. In this nomenclature, ''oxide traps'' are simply defects in the SiO 2 layer of the MOS structure, and ''interface traps'' are defects at the Si/SiO 2 interface. Nothing is presumed about how either type of defect communicates with the underlying Si. Electrically, ''fixed states'' are defined as trap levels that do not communicate with the Si on the time scale of the measurements, but ''switching states'' can exchange charge with the Si. Fixed states presumably are oxide traps in most types of measurements, but switching states can either be interface traps or near-interfacial oxide traps that can communicate with the Si, i.e., ''border traps'' [D. M. Fleetwood, IEEE Trans. Nucl. Sci. NS-39, 269 (1992)]. The effective density of border traps depends on the time scale and bias conditions of the measurements. We show the revised nomenclature can provide focus to discussions of the buildup and annealing of radiation-induced charge in non-radiation-hardened MOS transistors, and to changes in the 1/f noise of MOS devices through irradiation and elevated-temperature annealing

  14. Analysis of glycated hemoglobin A1c by capillary electrophoresis and capillary isoelectric focusing

    Czech Academy of Sciences Publication Activity Database

    Koval, Dušan; Kašička, Václav; Cottet, H.

    2011-01-01

    Roč. 413, č. 1 (2011), s. 8-15 ISSN 0003-2697 R&D Projects: GA ČR GP203/09/P485; GA ČR(CZ) GA203/08/1428 Institutional research plan: CEZ:AV0Z40550506 Keywords : capillary zone electrophoresis * capillary isoelectric focusing * glycated hemoglobin HbA1c Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.996, year: 2011

  15. Capillary optics for radiation focusing

    International Nuclear Information System (INIS)

    Peurrung, A.J.; Reeder, P.L.; Bliss, M.; Craig, R.A.; Lepel, E.A.; Stromswold, D.C.; Stoffels, J.; Sunberg, D.S.; Tenny, H.

    1996-11-01

    Capillary lens technology may ultimately bring benefits to neutron and x-ray-based science like conventional lenses with visible light. Although the technology is not yet 10 years old, these lenses have already had a significant impact in engineering, science, and medicine. Capillary lenses are advantageous when it is desirable to increase the radiation flux at a location without regard to its angular divergence. PNNL has worked to improve the technology in several ways. A single, optimally tapered capillary was manufactured, which allows intensity gains of a factor of 270 for an initially parallel, incident x-ray beam. Feasibility of constructing neutron lenses using 58 Ni (particularly effective at reflecting neutrons) has been explored. Three applications for capillary optics have been identified and studied: neutron telescope, Gandolphi x-ray diffractometry, and neutron radiotherapy. A brief guide is given for determining which potential applications are likely to be helped by capillary optics

  16. Engineering task plan for purged light system

    International Nuclear Information System (INIS)

    BOGER, R.M.

    1999-01-01

    A purged, closed circuit television system is currently used to video inside of waste tanks. The video is used to support inspection and assessment of the tank interiors, waste residues, and deployed hardware. The system is also used to facilitate deployment of new equipment. A new light source has been requested by Characterization Project Operations (CPO) for the video system. The current light used is mounted on the camera and provides 75 watts of light, which is insufficient for clear video. Other light sources currently in use on the Hanford site either can not be deployed in a 4-inch riser or do not meet the ignition source controls. The scope of this Engineering Task Plan is to address all activities associated with the specification and procurement of a light source for use with the existing CPO video equipment. The installation design change to tank farm facilities is not within the scope of this ETP

  17. Capillary waves of compressible fluids

    International Nuclear Information System (INIS)

    Falk, Kerstin; Mecke, Klaus

    2011-01-01

    The interplay of thermal noise and molecular forces is responsible for surprising features of liquids on sub-micrometer lengths-in particular at interfaces. Not only does the surface tension depend on the size of an applied distortion and nanoscopic thin liquid films dewet faster than would be expected from hydrodynamics, but also the dispersion relation of capillary waves differ at the nanoscale from the familiar macroscopic behavior. Starting with the stochastic Navier-Stokes equation we study the coupling of capillary waves to acoustic surface waves which is possible in compressible fluids. We find propagating 'acoustic-capillary waves' at nanometer wavelengths where in incompressible fluids capillary waves are overdamped.

  18. Determination of Wastewater Compounds in Sediment and Soil by Pressurized Solvent Extraction, Solid-Phase Extraction, and Capillary-Column Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Burkhardt, Mark R.; Zaugg, Steven D.; Smith, Steven G.; ReVello, Rhiannon C.

    2006-01-01

    A method for the determination of 61 compounds in environmental sediment and soil samples is described. The method was developed in response to increasing concern over the effects of endocrine-disrupting chemicals in wastewater and wastewater-impacted sediment on aquatic organisms. This method also may be used to evaluate the effects of combined sanitary and storm-sewer overflow on the water and sediment quality of urban streams. Method development focused on the determination of compounds that were chosen on the basis of their endocrine-disrupting potential or toxicity. These compounds include the alkylphenol ethoxylate nonionic surfactants and their degradates, food additives, fragrances, antioxidants, flame retardants, plasticizers, industrial solvents, disinfectants, fecal sterols, polycyclic aromatic hydrocarbons, and high-use domestic pesticides. Sediment and soil samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from interfering matrix components by high-pressure water/isopropyl alcohol extraction. The compounds were isolated using disposable solid-phase extraction (SPE) cartridges containing chemically modified polystyrene-divinylbenzene resin. The cartridges were dried with nitrogen gas, and then sorbed compounds were eluted with methylene chloride (80 percent)-diethyl ether (20 percent) through Florisil/sodium sulfate SPE cartridge, and then determined by capillary-column gas chromatography/mass spectrometry. Recoveries in reagent-sand samples fortified at 4 to 72 micrograms averaged 76 percent ?13 percent relative standard deviation for all method compounds. Initial method reporting levels for single-component compounds ranged from 50 to 500 micrograms per kilogram. The concentrations of 20 out of 61 compounds initially will be reported as estimated with the 'E' remark code for one of three reasons: (1) unacceptably low-biased recovery (less than 60 percent) or highly variable method performance

  19. Controlling retention, selectivity and magnitude of EOF by segmented monolithic columns consisting of octadecyl and naphthyl monolithic segments--applications to RP-CEC of both neutral and charged solutes.

    Science.gov (United States)

    Karenga, Samuel; El Rassi, Ziad

    2011-04-01

    Monolithic capillaries made of two adjoining segments each filled with a different monolith were introduced for the control and manipulation of the electroosmotic flow (EOF), retention and selectivity in reversed phase-capillary electrochromatography (RP-CEC). These columns were called segmented monolithic columns (SMCs) where one segment was filled with a naphthyl methacrylate monolith (NMM) to provide hydrophobic and π-interactions, while the other segment was filled with an octadecyl acrylate monolith (ODM) to provide solely hydrophobic interaction. The ODM segment not only provided hydrophobic interactions but also functioned as the EOF accelerator segment. The average EOF of the SMC increased linearly with increasing the fractional length of the ODM segment. The neutral SMC provided a convenient way for tuning EOF, selectivity and retention in the absence of annoying electrostatic interactions and irreversible solute adsorption. The SMCs allowed the separation of a wide range of neutral solutes including polycyclic aromatic hydrocarbons (PAHs) that are difficult to separate using conventional alkyl-bonded stationary phases. In all cases, the k' of a given solute was a linear function of the fractional length of the ODM or NMM segment in the SMCs, thus facilitating the tailoring of a given SMC to solve a given separation problem. At some ODM fractional length, the fabricated SMC allowed the separation of charged solutes such as peptides and proteins that could not otherwise be achieved on a monolithic column made from NMM as an isotropic stationary phase due to the lower EOF exhibited by this monolith. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Eco-friendly ionic liquid assisted capillary electrophoresis and α-acid glycoprotein-assisted liquid chromatography for simultaneous determination of anticancer drugs in human fluids.

    Science.gov (United States)

    Abd El-Hady, Deia; Albishri, Hassan M; Rengarajan, Rajesh

    2015-06-01

    In the current work, two eco-friendly analytical methods based on capillary electrophoresis (CE) and reversed phase liquid chromatography (RPLC) were developed for simultaneous determination of the most commonly used anticancer drugs for Hodgkin's disease: methotrexate (MTX), vinblastine, chlorambucil and dacarbazine. A background electrolyte (BGE) of 12.5 mmol/L phosphate buffer at pH 7.4 and 0.1 µmol/L 1-butyl-3-methyl imidazolium bromide (BMImBr) ionic liquid (IL) was used for CE measurements at 250 nm detection wavelength, 20 kV applied voltage and 25 °C. The rinsing protocol was significantly improved to reduce the adsorption of IL on the interior surface of capillary. Moreover, RPLC method was developed on α-1-acid glycoprotein (AGP) column. Mobile phase was 10 mmol/L phosphate buffer at pH 6.0 (100% v/v) and flow rate at 0.1 mL/min. As AGP is a chiral column, it was successfully separated l-MTX from its enantiomer impurity d-MTX. Good linearity of quantitative analysis was achieved with coefficients of determinations (r(2) ) >0.995. The stability of drugs measurements was investigated with adequate recoveries up to 24 h storage time under ambient temperature. The limits of detection were <50 and 90 ng/mL by CE and RPLC, respectively. The using of short-chain IL as an additive in BGE achieved 600-fold sensitivity enhancement compared with conventional Capillary Zone Electrophoresis (CZE). Therefore, for the first time, the proposed methods were successfully applied to determine simultaneously the analytes in human plasma and urine samples at clinically relevant concentrations with fast and simple pretreatments. Developed IL-assisted CE and RPLC methods were also applied to measure MTX levels in patients' samples over time. Copyright © 2014 John Wiley & Sons, Ltd.

  1. Nasal Lobular Capillary Hemangioma

    Directory of Open Access Journals (Sweden)

    Prashant Patil

    2013-01-01

    Full Text Available Nasal lobular capillary hemangioma is a rare benign tumor of the paranasal sinuses. This lesion is believed to grow rapidly in size over time. The exact etiopathogenesis is still a dilemma. We discuss a case of nasal lobular capillary hemangioma presenting with a history of epistaxis. Contrast enhanced computed tomography of paranasal sinuses revealed an intensely enhancing soft-tissue mass in the left nasal cavity and left middle and inferior meati with no obvious bony remodeling or destruction. We present imaging and pathologic features of nasal lobular capillary hemangioma and differentiate it from other entities like nasal angiofibroma.

  2. Numerical study on flow rate limitation of open capillary channel flow through a wedge

    Directory of Open Access Journals (Sweden)

    Ting-Ting Zhang

    2016-04-01

    Full Text Available The flow characteristics of slender-column flow in wedge-shaped channel under microgravity condition are investigated in this work. The one-dimensional theoretical model is applied to predict the critical flow rate and surface contour of stable flow. However, the one-dimensional model overestimates the critical flow rate for not considering the extra pressure loss. Then, we develop a three-dimensional simulation method with OpenFOAM, a computational fluid dynamics tool, to simulate various phenomena in wedge channels with different lengths. The numerical results are verified with the capillary channel flow experimental data on the International Space Station. We find that the three-dimensional simulation perfectly predicts the critical flow rates and surface contours under various flow conditions. Meanwhile, the general behaviors in subcritical, critical, and supercritical flow are studied in three-dimensional simulation considering variations of flow rate and open channel length. The numerical techniques for three-dimensional simulation is validated for a wide range of configurations and is hopeful to provide valuable guidance for capillary channel flow experiment and efficient liquid management in space.

  3. Experimental and numerical studies of choked flow through adiabatic and diabatic capillary tubes

    International Nuclear Information System (INIS)

    Deodhar, Subodh D.; Kothadia, Hardik B.; Iyer, K.N.; Prabhu, S.V.

    2015-01-01

    Capillary tubes are extensively used in several cooling applications like refrigeration, electronic cooling etc. Local pressure variation in adiabatic straight capillary tube (mini channel) is studied experimentally and numerically with R134a as the working fluid. Experiments are performed on two straight capillary tubes. It is found that the diameter is the most sensitive design parameter of the capillary tube. Experiments are performed on five helically coiled capillary tubes to quantify the effect of pitch and curvature of helically coiled capillary tube on the pressure drop. Non dimensionalized factor to account coiling of capillary tube is derived to calculate mass flow rate in helically coiled capillary tubes. Flow visualization in adiabatic capillary tube confirms the bubbly nature of two phase flow. Numerical and experimental investigations in diabatic capillary tube suggest that the use of positive displacement pump and choking at the exit of the channel ensures flow stability. - Highlights: • Model is developed to design capillary tube in adiabatic and diabatic condition. • Effect of coil curvature on pressure drop is studied experimentally. • Correlation is developed to predict mass flow rate in helical capillary tubes. • Flow visualization is carried out to check the type of two phase flow. • Effect of choked flow on diabatic capillary tubes is studied experimentally.

  4. On hydraulics of capillary tubes

    Directory of Open Access Journals (Sweden)

    N.G. Aloyan

    2016-03-01

    Full Text Available The article considers the laws of motion of water in the capillary tubes, taken as a model for flowing well, on the analogical net count device. For capillary tube the lower limit value of flow rate is empirically determined above which the total hydraulic resistance of the capillary is practically constant. The specificity of the phenomenon is that the regime of motion, by a Reynolds number, for a given flow rate still remains laminar. This circumstance can perplex the specialists, so the author invites them to the scientific debate on the subject of study. Obviously, to identify the resulting puzzle it is necessary to conduct a series of experiments using capillaries of different lengths and diameters and with different values of overpressure. The article states that in tubes with very small diameter the preliminary magnitude of capillary rise of water in the presence of flow plays no role and can be neglected.

  5. Western blotting using capillary electrophoresis.

    Science.gov (United States)

    Anderson, Gwendolyn J; M Cipolla, Cynthia; Kennedy, Robert T

    2011-02-15

    A microscale Western blotting system based on separating sodium-dodecyl sulfate protein complexes by capillary gel electrophoresis followed by deposition onto a blotting membrane for immunoassay is described. In the system, the separation capillary is grounded through a sheath capillary to a mobile X-Y translation stage which moves a blotting membrane past the capillary outlet for protein deposition. The blotting membrane is moistened with a methanol and buffer mixture to facilitate protein adsorption. Although discrete protein zones could be detected, bands were broadened by ∼1.7-fold by transfer to membrane. A complete Western blot for lysozyme was completed in about one hour with 50 pg mass detection limit from low microgram per milliliter samples. These results demonstrate substantial reduction in time requirements and improvement in mass sensitivity compared to conventional Western blots. Western blotting using capillary electrophoresis shows promise to analyze low volume samples with reduced reagents and time, while retaining the information content of a typical Western blot.

  6. Progression of Diabetic Capillary Occlusion: A Model.

    Directory of Open Access Journals (Sweden)

    Xiao Fu

    2016-06-01

    Full Text Available An explanatory computational model is developed of the contiguous areas of retinal capillary loss which play a large role in diabetic maculapathy and diabetic retinal neovascularization. Strictly random leukocyte mediated capillary occlusion cannot explain the occurrence of large contiguous areas of retinal ischemia. Therefore occlusion of an individual capillary must increase the probability of occlusion of surrounding capillaries. A retinal perifoveal vascular sector as well as a peripheral retinal capillary network and a deleted hexagonal capillary network are modelled using Compucell3D. The perifoveal modelling produces a pattern of spreading capillary loss with associated macular edema. In the peripheral network, spreading ischemia results from the progressive loss of the ladder capillaries which connect peripheral arterioles and venules. System blood flow was elevated in the macular model before a later reduction in flow in cases with progression of capillary occlusions. Simulations differing only in initial vascular network structures but with identical dynamics for oxygen, growth factors and vascular occlusions, replicate key clinical observations of ischemia and macular edema in the posterior pole and ischemia in the retinal periphery. The simulation results also seem consistent with quantitative data on macular blood flow and qualitative data on venous oxygenation. One computational model applied to distinct capillary networks in different retinal regions yielded results comparable to clinical observations in those regions.

  7. RPLC-lon-trap-FTMS method for lipid profiling of plasma: Method validation And application to p53 mutant mouse model

    NARCIS (Netherlands)

    Hu, C.; Dommelen, J. van; Heijden, R. van der; Spijksma, G.; Reijmers, T.H.; Wang, M.; Slee, E.; Lu, X.; Xu, G.; Greef, J. van der; Hankemeier, T.

    2008-01-01

    A reversed-phase liquid chromatography-linear ion trap-Fourier transform ion cyclotron resonance-mass spectrometry method was developed for the profiling of lipids in human and mouse plasma. With the use of a fused-core C8 column and a binary gradient, more than 160 lipids belonging to

  8. Fluid Delivery System For Capillary Electrophoretic Applications.

    Science.gov (United States)

    Li, Qingbo; Liu, Changsheng; Kane, Thomas E.; Kernan, John R.; Sonnenschein, Bernard; Sharer, Michael V.

    2002-04-23

    An automated electrophoretic system is disclosed. The system employs a capillary cartridge having a plurality of capillary tubes. The cartridge has a first array of capillary ends projecting from one side of a plate. The first array of capillary ends are spaced apart in substantially the same manner as the wells of a microtitre tray of standard size. This allows one to simultaneously perform capillary electrophoresis on samples present in each of the wells of the tray. The system includes a stacked, dual carrousel arrangement to eliminate cross-contamination resulting from reuse of the same buffer tray on consecutive executions from electrophoresis. The system also has a gel delivery module containing a gel syringe/a stepper motor or a high pressure chamber with a pump to quickly and uniformly deliver gel through the capillary tubes. The system further includes a multi-wavelength beam generator to generate a laser beam which produces a beam with a wide range of wavelengths. An off-line capillary reconditioner thoroughly cleans a capillary cartridge to enable simultaneous execution of electrophoresis with another capillary cartridge. The streamlined nature of the off-line capillary reconditioner offers the advantage of increased system throughput with a minimal increase in system cost.

  9. Capillary electrophoresis: principles and applications in illicit drug analysis.

    Science.gov (United States)

    Tagliaro, F; Turrina, S; Smith, F P

    1996-02-09

    Capillary electrophoresis, which appeared in the early 1980s, is now rapidly expanding into many scientific disciplines, including analytical chemistry, biotechnology and biomedical and pharmaceutical sciences. In capillary electrophoresis,electrokinetic separations are carried out in tiny capillaries at high voltages (10-30 kV), thus obtaining high efficiencies (N > 10(5)) and excellent mass sensitivities (down to 10(-18)-10(-20) moles). The main features of capillary electrophoresis are: versatility of application (from inorganic ions to large DNA fragments), use of different separation modes with different selectivity, extremely low demands on sample volume, negligible running costs, possibility of interfacing with different detection systems, ruggedness and simplicity of instrumentation. Capillary electrophoresis applications in forensic sciences have appeared only recently, but are now rapidly growing, particularly in forensic toxicology. The present paper briefly describes the basic principles of capillary electrophoresis, from both the instrumental and analytical points of view. Furthermore, the main applications in the analysis of illicit/controlled drugs in both illicit preparations and biological samples are presented and discussed (43 references). It is concluded that the particular separation mechanism and the high complementarity of this technique to chromatography makes capillary electrophoresis a new powerful tool of investigation in the hands of forensic toxicologists.

  10. Vertically averaged approaches for CO 2 migration with solubility trapping

    KAUST Repository

    Gasda, S. E.

    2011-05-20

    The long-term storage security of injected carbon dioxide (CO2) is an essential component of geological carbon sequestration operations. In the postinjection phase, the mobile CO2 plume migrates in large part because of buoyancy forces, following the natural topography of the geological formation. The primary trapping mechanisms are capillary and solubility trapping, which evolve over hundreds to thousands of years and can immobilize a significant portion of the mobile CO2 plume. However, both the migration and trapping processes are inherently complex, spanning multiple spatial and temporal scales. Using an appropriate model that can capture both large- and small-scale effects is essential for understanding the role of these processes on the long-term storage security of CO2 sequestration operations. Traditional numerical models quickly become prohibitively expensive for the type of large-scale, long-term modeling that is necessary for characterizing the migration and immobilization of CO2 during the postinjection period. We present an alternative modeling option that combines vertically integrated governing equations with an upscaled representation of the dissolution-convection process. With this approach, we demonstrate the effect of different modeling choices for typical large-scale geological systems and show that practical calculations can be performed at the temporal and spatial scales of interest. Copyright 2011 by the American Geophysical Union.

  11. Investigation of transient dynamics of capillary assisted particle assembly yield

    Energy Technology Data Exchange (ETDEWEB)

    Virganavičius, D. [Institute of Materials Science, Kaunas University of Technology, K. Baršausko St. 59, Kaunas LT-51423 (Lithuania); Laboratory of Micro- and Nanotechnology, Paul Scherrer Institut, 5232 Villigen PSI (Switzerland); Juodėnas, M. [Institute of Materials Science, Kaunas University of Technology, K. Baršausko St. 59, Kaunas LT-51423 (Lithuania); Tamulevičius, T., E-mail: tomas.tamulevicius@ktu.lt [Institute of Materials Science, Kaunas University of Technology, K. Baršausko St. 59, Kaunas LT-51423 (Lithuania); Department of Physics, Kaunas University of Technology, Studentų St. 50, Kaunas LT-51368 (Lithuania); Schift, H. [Laboratory of Micro- and Nanotechnology, Paul Scherrer Institut, 5232 Villigen PSI (Switzerland); Tamulevičius, S. [Institute of Materials Science, Kaunas University of Technology, K. Baršausko St. 59, Kaunas LT-51423 (Lithuania); Department of Physics, Kaunas University of Technology, Studentų St. 50, Kaunas LT-51368 (Lithuania)

    2017-06-01

    Highlights: • Regular particles arrays were assembled by capillary force assisted deposition. • Deposition yield dynamics was investigated at different thermal velocity regimes. • Yield transient behavior was approximated with logistic function. • Pattern density influence for switching behavior was assessed. - Abstract: In this paper, the transient behavior of the particle assembly yield dynamics when switching from low yield to high yield deposition at different velocity and thermal regimes is investigated. Capillary force assisted particle assembly (CAPA) using colloidal suspension of green fluorescent 270 nm diameter polystyrene beads was performed on patterned poly (dimethyl siloxane) substrates using a custom-built deposition setup. Two types of patterns with different trapping site densities were used to assess CAPA process dynamics and the influence of pattern density and geometry on the deposition yield transitions. Closely packed 300 nm diameter circular pits ordered in hexagonal arrangement with 300 nm pitch, and 2 × 2 mm{sup 2} square pits with 2 μm spacing were used. 2-D regular structures of the deposited particles were investigated by means of optical fluorescence and scanning electron microscopy. The fluorescence micrographs were analyzed using a custom algorithm enabling to identify particles and calculate efficiency of the deposition performed at different regimes. Relationship between the spatial distribution of particles in transition zone and ambient conditions was evaluated and quantified by approximation of the yield profile with a logistic function.

  12. Rapid capillary coating by epoxy-poly-(dimethylacrylamide): Performance in capillary zone electrophoresis of protein and polystyrene carboxylate

    Czech Academy of Sciences Publication Activity Database

    Chiari, M.; Cretich, M.; Šťastná, Miroslava; Radko, S. P.; Chrambach, A.

    2001-01-01

    Roč. 22, č. 4 (2001), s. 656-659 ISSN 0173-0835 Institutional research plan: CEZ:AV0Z4031919 Keywords : capillary coating * capillary zone electrophoresis * proteins Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.282, year: 2001

  13. Identification and olfactometry of French fries flavour extracted at mouth conditions

    NARCIS (Netherlands)

    Posthumus, M.A.; Loon, W.A.M.; Linssen, J.P.H.; Legger, A.; Voragen, A.G.J.

    2005-01-01

    The aim of this study was to isolate and identify odour active compounds from French fries at mouth conditions. Volatile compounds were released from French fries by purge-and-trap, trapped on Tenax TA, and identified with GC–MS. GC–olfactometry was used to determine odour active compounds with a

  14. Condensation and Evaporation Transitions in Deep Capillary Grooves

    OpenAIRE

    Malijevský, A. (Alexandr); Parry, A.O.

    2014-01-01

    We study the order of capillary condensation and evaporation transitions of a simple fluid adsorbed in a deep capillary groove using a fundamental measure density functional theory (DFT). The walls of the capillary interact with the fluid particles via long-ranged, dispersion, forces while the fluid-fluid interaction is modelled as a truncated Lennard-Jones-like potential. We find that below the wetting temperature $T_w$ condensation is first-order and evaporation is continuous with the metas...

  15. Method for determination of methyl tert-butyl ether and its degradation products in water

    Science.gov (United States)

    Church, C.D.; Isabelle, L.M.; Pankow, J.F.; Rose, D.L.; Tratnyek, P.G.

    1997-01-01

    An analytical method is described that can detect the major alkyl ether compounds that are used as gasoline oxygenates (methyl tert-butyl ether, MTBE; ethyl tert-butyl ether, ETBE; and tert-amyl methyl ether, TAME) and their most characteristic degradation products (tert-butyl alcohol, TBA; tert-butyl formate, TBF; and tert-amyl alcohol, TAA) in water at sub-ppb concentrations. The new method involves gas chromatography (GC) with direct aqueous injection (DAI) onto a polar column via a splitless injector, coupled with detection by mass spectrometry (MS). DAI-GC/MS gives excellent agreement with conventional purge-and-trap methods for MTBE over a wide range of environmentally relevant concentrations. The new method can also give simultaneous identification of polar compounds that might occur as degradation products of gasoline oxygenates, such as TBA, TBF, TAA, methyl acetate, and acetone. When the method was applied to effluent from a column microcosm prepared with core material from an urban site in New Jersey, conversion of MTBE to TBA was observed after a lag period of 35 days. However, to date, analyses of water samples from six field sites using the DAI-GC/MS method have not produced evidence for the expected products of in situ degradation of MTBE.An analytical method is described that can detect the major alkyl ether compounds that are used as gasoline oxygenates (methyl tert-butyl ether, MTBE; ethyl tert-butyl ether, ETBE; and tert-amyl methyl ether, TAME) and their most characteristic degradation products (tert-butyl alcohol, TBA; tert-butyl formate, TBF; and tert-amyl alcohol, TAA) in water at sub-ppb concentrations. The new method involves gas chromatography (GC) with direct aqueous injection (DAI) onto a polar column via a splitless injector, coupled with detection by mass spectrometry (MS). DAI-GC/MS gives excellent agreement with conventional purge-and-trap methods for MTBE over a wide range of environmentally relevant concentrations. The new method

  16. The loss of essential oil components induced by the Purge Time in the Pressurized Liquid Extraction (PLE) procedure of Cupressus sempervirens.

    Science.gov (United States)

    Dawidowicz, Andrzej L; Czapczyńska, Natalia B; Wianowska, Dorota

    2012-05-30

    The influence of different Purge Times on the effectiveness of Pressurized Liquid Extraction (PLE) of volatile oil components from cypress plant matrix (Cupressus sempervirens) was investigated, applying solvents of diverse extraction efficiencies. The obtained results show the decrease of the mass yields of essential oil components as a result of increased Purge Time. The loss of extracted components depends on the extrahent type - the greatest mass yield loss occurred in the case of non-polar solvents, whereas the smallest was found in polar extracts. Comparisons of the PLE method with Sea Sand Disruption Method (SSDM), Matrix Solid-Phase Dispersion Method (MSPD) and Steam Distillation (SD) were performed to assess the method's accuracy. Independent of the solvent and Purge Time applied in the PLE process, the total mass yield was lower than the one obtained for simple, short and relatively cheap low-temperature matrix disruption procedures - MSPD and SSDM. Thus, in the case of volatile oils analysis, the application of these methods is advisable. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Discriminating between antihydrogen and mirror-trapped antiprotons in a minimum-B trap

    CERN Document Server

    Amole, C; Ashkezari, M D; Baquero-Ruiz, M; Bertsche, W; Butler, E; Cesar, C L; Chapman, S; Charlton, M; Deller, A; Eriksson, S; Fajans, J; Friesen, T; Fujiwara, M C; Gill, D R; Gutierrez, A; Hangst, J S; Hardy, W N; Hayden, M E; Humphries, A J; Hydomako, R; Kurchaninov, L; Jonsell, S; Madsen, N; Menary, S; Nolan, P; Olchanski, K; Olin, A; Povilus, A; Pusa, P; Robicheaux, F; Sarid, E; Silveira, D M; So, C; Storey, J W; Thompson, R I; van der Werf, D P; Wurtele, J S

    2012-01-01

    Recently, antihydrogen atoms were trapped at CERN in a magnetic minimum (minimum-B) trap formed by superconducting octupole and mirror magnet coils. The trapped antiatoms were detected by rapidly turning off these magnets, thereby eliminating the magnetic minimum and releasing any antiatoms contained in the trap. Once released, these antiatoms quickly hit the trap wall, whereupon the positrons and antiprotons in the antiatoms annihilated. The antiproton annihilations produce easily detected signals; we used these signals to prove that we trapped antihydrogen. However, our technique could be confounded by mirror-trapped antiprotons, which would produce seemingly-identical annihilation signals upon hitting the trap wall. In this paper, we discuss possible sources of mirror-trapped antiprotons and show that antihydrogen and antiprotons can be readily distinguished, often with the aid of applied electric fields, by analyzing the annihilation locations and times. We further discuss the general properties of antipr...

  18. DNA typing by capillary electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, N.

    1997-10-08

    Capillary electrophoresis is becoming more and more important in nucleic acid analysis including DNA sequencing, typing and disease gene measurements. This work summarized the background of DNA typing. The recent development of capillary electrophoresis was also discussed. The second part of the thesis showed the principle of DNA typing based on using the allelic ladder as the absolute standard ladder in capillary electrophoresis system. Future work will be focused on demonstrating DNA typing on multiplex loci and examples of disease diagnosis in the on-line format of PCR-CE. Also capillary array electrophoresis system should allow high throughput, fast speed DNA typing. Only the introduction and conclusions for this report are available here. A reprint was removed for separate processing.

  19. Insights into head-column field-amplified sample stacking: Part II. Study of the behavior of the electrophoretic system after electrokinetic injection of cationic compounds across a short water plug

    Czech Academy of Sciences Publication Activity Database

    Šesták, Jozef; Thormann, W.

    2017-01-01

    Roč. 1512, AUG (2017), s. 124-132 ISSN 0021-9673 Institutional support: RVO:68081715 Keywords : head-column field-amplified sample stacking * capillary electrophoresis * water plug Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 3.981, year: 2016

  20. Insights into head-column field-amplified sample stacking: Part II. Study of the behavior of the electrophoretic system after electrokinetic injection of cationic compounds across a short water plug

    Czech Academy of Sciences Publication Activity Database

    Šesták, Jozef; Thormann, W.

    2017-01-01

    Roč. 1512, AUG (2017), s. 124-132 ISSN 0021-9673 Institutional support: RVO:68081715 Keywords : head- column field-amplified sample stacking * capillary electrophoresis * water plug Subject RIV: CB - Analytical Chemistry, Separation OBOR OECD: Analytical chemistry Impact factor: 3.981, year: 2016

  1. Capillary-Condenser-Pumped Heat-Transfer Loop

    Science.gov (United States)

    Silverstein, Calvin C.

    1989-01-01

    Heat being transferred supplies operating power. Capillary-condenser-pumped heat-transfer loop similar to heat pipe and to capillary-evaporator-pumped heat-transfer loop in that heat-transfer fluid pumped by evaporation and condensation of fluid at heat source and sink, respectively. Capillary condenser pump combined with capillary evaporator pump to form heat exchanger circulating heat-transfer fluids in both loops. Transport of heat more nearly isothermal. Thermal stress in loop reduced, and less external surface area needed in condenser section for rejection of heat to heat sink.

  2. 50 CFR 697.19 - Trap limits and trap tag requirements for vessels fishing with lobster traps.

    Science.gov (United States)

    2010-10-01

    ... vessels fishing with lobster traps. 697.19 Section 697.19 Wildlife and Fisheries FISHERY CONSERVATION AND... requirements for vessels fishing with lobster traps. (a) Trap limits for vessels fishing or authorized to fish... management area designation certificate or valid limited access American lobster permit specifying one or...

  3. Capillary Condensation in Confined Media

    OpenAIRE

    Charlaix, Elisabeth; Ciccotti, Matteo

    2009-01-01

    28 pages - To appear in 2010 in the Handbook of Nanophysics - Vol 1 - Edited by Klaus Sattler - CRC Press; We review here the physics of capillary condensation of liquids in confined media, with a special regard to the application in nanotechnologies. The thermodynamics of capillary condensation and thin film adsorption are first exposed along with all the relevant notions. The focus is then shifted to the modelling of capillary forces, to their measurements techniques (including SFA, AFM and...

  4. Comprehensive protein profiling by multiplexed capillary zone electrophoresis using cross-linked polyacrylamide coated capillaries.

    Science.gov (United States)

    Liu, Shaorong; Gao, Lin; Pu, Qiaosheng; Lu, Joann J; Wang, Xingjia

    2006-02-01

    We have recently developed a new process to create cross-linked polyacrylamide (CPA) coatings on capillary walls to suppress protein-wall interactions. Here, we demonstrate CPA-coated capillaries for high-efficiency (>2 x 10(6) plates per meter) protein separations by capillary zone electrophoresis (CZE). Because CPA virtually eliminates electroosmotic flow, positive and negative proteins cannot be analyzed in a single run. A "one-sample-two-separation" approach is developed to achieve a comprehensive protein analysis. High throughput is achieved through a multiplexed CZE system.

  5. Bacterial surface layer proteins as a novel capillary coating material for capillary electrophoretic separations

    Energy Technology Data Exchange (ETDEWEB)

    Moreno-Gordaliza, Estefanía, E-mail: emorenog@ucm.es [Division of Analytical Biosciences, Leiden Academic Centre for Drug Research, Universiteit Leiden, Einsteinweg 55, 2300, RA, Leiden (Netherlands); Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, Avda. Complutense s/n, 28040, Madrid (Spain); Stigter, Edwin C.A. [Division of Analytical Biosciences, Leiden Academic Centre for Drug Research, Universiteit Leiden, Einsteinweg 55, 2300, RA, Leiden (Netherlands); Department of Molecular Cancer Research, Universitair Medisch Centrum Utrecht, Wilhelmina Kinder Ziekenhuis, Lundlaan 6, 3584, EA Utrecht (Netherlands); Lindenburg, Petrus W.; Hankemeier, Thomas [Division of Analytical Biosciences, Leiden Academic Centre for Drug Research, Universiteit Leiden, Einsteinweg 55, 2300, RA, Leiden (Netherlands)

    2016-06-07

    A novel concept for stable coating in capillary electrophoresis, based on recrystallization of surface layer proteins on hydrophobized fused silica capillaries, was demonstrated. Surface layer protein A (SlpA) from Lactobacillus acidophilus bacteria was extracted, purified and used for coating pre-silanized glass substrates presenting different surface wettabilities (either hydrophobic or hydrophilic). Contact angle determination on SlpA-coated hydrophobic silica slides showed that the surfaces turned to hydrophilic after coating (53 ± 5°), due to a protein monolayer formation by protein-surface hydrophobic interactions. Visualization by atomic force microscopy demonstrated the presence of a SlpA layer on methylated silica slides displaying a surface roughness of 0.44 ± 0.02 nm. Additionally, a protein layer was visualized by fluorescence microscopy in methylated silica capillaries coated with SlpA and fluorescein isothiocyanate-labeled. The SlpA-coating showed an outstanding stability, even after treatment with 20 mM NaOH (pH 12.3). The electroosmotic flow in coated capillaries showed a partial suppression at pH 7.50 (3.8 ± 0.5 10{sup −9} m{sup 2} V{sup −1} s{sup −1}) when compared with unmodified fused silica (5.9 ± 0.1 10{sup −8} m{sup 2} V{sup −1} s{sup −1}). To demonstrate the potential of this novel coating, the SlpA-coated capillaries were applied for the first time for electrophoretic separation, and proved to be very suitable for the isotachophoretic separation of lipoproteins in human serum. The separations showed a high degree of repeatability (absolute migration times with 1.1–1.8% coefficient-of-variation (CV) within a day) and 2–3% CV inter-capillary reproducibility. The capillaries were stable for more than 100 runs at pH 9.40, and showed to be an exceptional alternative for challenging electrophoretic separations at long-term use. - Highlights: • New coating using recrystallized surface-layer proteins on

  6. Understanding and diminishing the extra-column band broadening effects in supercritical fluid chromatography.

    Science.gov (United States)

    De Pauw, Ruben; Shoykhet Choikhet, Konstantin; Desmet, Gert; Broeckhoven, Ken

    2015-07-17

    Supercritical fluid chromatography, where a low-viscosity mobile phase such as carbon dioxide is used, proves to be an excellent technique for fast and efficient separations, especially when sub-2μm particles are used. However, to achieve high velocities when using these small particles, and in order to stay within the flow rate range of current SFC-instruments, narrow columns (e.g. 2.1mm ID) must be used. Unfortunately, state-of-the-art instrumentation is limiting the full separation power of these narrower columns due to significant extra-column band broadening effects. The present work identifies and quantifies the different contributions to extra-column band broadening in SFC such as the influence of the sample solvent, injection volume, extra-column volumes and detector cell volume/design. When matching the sample solvent to the mobile phase in terms of elution strength and polarity (e.g. using hexane/ethanol/isopropanol 85/10/5vol%) and lowering the injection volume to 0.4μL, the plate count can be increased from 7600 to 21,300 for a low-retaining compound (k'=2.3) on a 2.1mm×150mm column (packed with 1.8μm particles). The application of a water/acetonitrile mixture as sample solvent was also investigated. It was found that when the volumetric ratio of water/acetonitrile was optimized, only a slightly lower plate count was measured compared to the hexane-based solvent when minimizing injection and extra-column volume. This confirms earlier results that water/acetonitrile can be used if water-soluble samples are considered or when a less volatile solvent is preferred. Minimizing the ID of the connection capillaries from 250 to 65μm, however, gives no further improvement in obtained efficiency for early-eluting compounds when a standard system configuration with optimized sample solvent was used. When switching to a state-of-the-art detector design with reduced (dispersion) volume (1.7-0.6μL), an increase in plate count is observed (from 11,000 to 14

  7. Channeling of neutral particles in micro- and nano-capillaries

    International Nuclear Information System (INIS)

    Dabagov, S.B.

    2003-01-01

    After briefly reviewing the main directions in X-ray optics and analyzing the development of capillary optics, a general theory of radiation propagation through capillary structures is described in both geometrical optics and wave optics approximations. Analysis of radiation field structure inside a capillary waveguide shows that wave propagation in channels can be of a purely modal nature, with transmitted energy mostly concentrated in the immediate neighbourhood of capillary inner walls. A qualitative change in radiation scattering with decreasing channel diameter 0 namely, the transition from surface channeling in microcapillaries to bulk channeling in nanocapillaries - is discussed [ru

  8. Digital microfluidics platform for interfacing solid-liquid extraction column with portable capillary electropherograph for analysis of soil amino acids.

    Science.gov (United States)

    Gorbatsova, Jelena; Jaanus, Martin; Vaher, Merike; Kaljurand, Mihkel

    2016-02-01

    In this work, the concept of a field-portable analyzer is proposed that operates with milliliter amounts of solvents and samples. The need to develop such an analyzer is not only driven by specific extraterrestrial analysis but also, for example, by forensics applications where the amount of liquid that can be taken to the field is severely limited. The prototype of the proposed analyzer consists of a solid-liquid extractor, the output of which is connected to the micropump, which delivers droplets of extracts to digital microfluidic platform (DMFP). In this way, world-to-chip interfacing is established. Further, the sample droplets are transported to CE capillary inlet port, separated and detected via a contactless conductivity detector. Working buffers and other solvents needed to perform CE analysis are also delivered as droplets to the DMFP and transported through the CE capillary. The performance of the analyzer is demonstrated by analysis of amino acids in sand matrices. The recovery of the spiked amino acids from the inert sand sample was from 34 to 51% with analysis LOD from 0.2 to 0.6 ppm and migration time RSD from 0.2 to 6.0%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Temperature-assisted solute focusing with sequential trap/release zones in isocratic and gradient capillary liquid chromatography: Simulation and experiment

    Science.gov (United States)

    Groskreutz, Stephen R.; Weber, Stephen G.

    2016-01-01

    In this work we characterize the development of a method to enhance temperature-assisted on-column solute focusing (TASF) called two-stage TASF. A new instrument was built to implement two-stage TASF consisting of a linear array of three independent, electronically controlled Peltier devices (thermoelectric coolers, TECs). Samples are loaded onto the chromatographic column with the first two TECs, TEC A and TEC B, cold. In the two-stage TASF approach TECs A and B are cooled during injection. TEC A is heated following sample loading. At some time following TEC A’s temperature rise, TEC B’s temperature is increased from the focusing temperature to a temperature matching that of TEC A. Injection bands are focused twice on-column, first on the initial TEC, e.g. single-stage TASF, then refocused on the second, cold TEC. Our goal is to understand the two-stage TASF approach in detail. We have developed a simple yet powerful digital simulation procedure to model the effect of changing temperature in the two focusing zones on retention, band shape and band spreading. The simulation can predict experimental chromatograms resulting from spatial and temporal temperature programs in combination with isocratic and solvent gradient elution. To assess the two-stage TASF method and the accuracy of the simulation well characterized solutes are needed. Thus, retention factors were measured at six temperatures (25–75 °C) at each of twelve mobile phases compositions (0.05–0.60 acetonitrile/water) for homologs of n-alkyl hydroxylbenzoate esters and n-alkyl p-hydroxyphenones. Simulations accurately reflect experimental results in showing that the two-stage approach improves separation quality. For example, two-stage TASF increased sensitivity for a low retention solute by a factor of 2.2 relative to single-stage TASF and 8.8 relative to isothermal conditions using isocratic elution. Gradient elution results for two-stage TASF were more encouraging. Application of two-stage TASF

  10. Imbibition of ``Open Capillary'': Fundamentals and Applications

    Science.gov (United States)

    Tani, Marie; Kawano, Ryuji; Kamiya, Koki; Okumura, Ko

    2015-11-01

    Control or transportation of small amount of liquid is one of the most important issues in various contexts including medical sciences or pharmaceutical industries to fuel delivery. We studied imbibition of ``open capillary'' both experimentally and theoretically, and found simple scaling laws for both statics and dynamics of the imbibition, similarly as that of imbibition of capillary tubes. Furthermore, we revealed the existence of ``precursor film,'' which developed ahead of the imbibing front, and the dynamics of it is described well by another scaling law for capillary rise in a corner. Then, to show capabilities of open capillaries, we demonstrated two experiments by fabricating micro mixing devices to achieve (1) simultaneous multi-color change of the Bromothymol blue (BTB) solution and (2) expression of the green florescent protein (GFP). This research was partly supported by ImPACT Program of Council for Science, Technology and Innovation (Cabinet Office, Government of Japan). M. T. is supported by the Japan Society for the Promotion of Science Research Fellowships for Young Scientists.

  11. Development of immobilized membrane-based affinity columns for use in the online characterization of membrane bound proteins and for targeted affinity isolations

    International Nuclear Information System (INIS)

    Moaddel, Ruin; Wainer, Irving W.

    2006-01-01

    Membranes obtained from cell lines that express or do not express a target membrane bound protein have been immobilized on a silica-based liquid chromatographic support or on the surface of an activated glass capillary. The resulting chromatographic columns have been placed in liquid chromatographic systems and used to characterize the target proteins and to identify small molecules that bind to the target. Membranes containing ligand gated ion channels, G-protein coupled receptors and drug transporters have been prepared and characterized. If a marker ligand has been identified for the target protein, frontal or zonal displacement chromatographic techniques can be used to determine binding affinities (K d values) and non-linear chromatography can be used to assess the association (k on ) and dissociation (k off ) rate constants and the thermodynamics of the binding process. Membrane-based affinity columns have been created using membranes from a cell line that does not express the target protein (control) and the same cell line that expresses the target protein (experimental) after genomic transfection. The resulting columns can be placed in a parallel chromatography system and the differential retention between the control and experimental columns can be used to identify small molecules and protein that bind to the target protein. These applications will be illustrated using columns created using cellular membranes containing nicotinic acetylcholine receptors and the drug transporter P-glycoprotein

  12. Development of immobilized membrane-based affinity columns for use in the online characterization of membrane bound proteins and for targeted affinity isolations

    Energy Technology Data Exchange (ETDEWEB)

    Moaddel, Ruin [Gerontology Research Center, National Institute on Aging, National Institutes of Health, 5600 Nathan Shock Drive, Baltimore, MD 21224-6825 (United States); Wainer, Irving W. [Gerontology Research Center, National Institute on Aging, National Institutes of Health, 5600 Nathan Shock Drive, Baltimore, MD 21224-6825 (United States)]. E-mail: Wainerir@grc.nia.nih.gov

    2006-03-30

    Membranes obtained from cell lines that express or do not express a target membrane bound protein have been immobilized on a silica-based liquid chromatographic support or on the surface of an activated glass capillary. The resulting chromatographic columns have been placed in liquid chromatographic systems and used to characterize the target proteins and to identify small molecules that bind to the target. Membranes containing ligand gated ion channels, G-protein coupled receptors and drug transporters have been prepared and characterized. If a marker ligand has been identified for the target protein, frontal or zonal displacement chromatographic techniques can be used to determine binding affinities (K {sub d} values) and non-linear chromatography can be used to assess the association (k {sub on}) and dissociation (k {sub off}) rate constants and the thermodynamics of the binding process. Membrane-based affinity columns have been created using membranes from a cell line that does not express the target protein (control) and the same cell line that expresses the target protein (experimental) after genomic transfection. The resulting columns can be placed in a parallel chromatography system and the differential retention between the control and experimental columns can be used to identify small molecules and protein that bind to the target protein. These applications will be illustrated using columns created using cellular membranes containing nicotinic acetylcholine receptors and the drug transporter P-glycoprotein.

  13. Trapping, self-trapping and the polaron family

    International Nuclear Information System (INIS)

    Stoneham, A M; Gavartin, J; Shluger, A L; Kimmel, A V; Ramo, D Munoz; Roennow, H M; Aeppli, G; Renner, C

    2007-01-01

    The earliest ideas of the polaron recognized that the coupling of an electron to ionic vibrations would affect its apparent mass and could effectively immobilize the carrier (self-trapping). We discuss how these basic ideas have been generalized to recognize new materials and new phenomena. First, there is an interplay between self-trapping and trapping associated with defects or with fluctuations in an amorphous solid. In high dielectric constant oxides, like HfO 2 , this leads to oxygen vacancies having as many as five charge states. In colossal magnetoresistance manganites, this interplay makes possible the scanning tunnelling microscopy (STM) observation of polarons. Second, excitons can self-trap and, by doing so, localize energy in ways that can modify the material properties. Third, new materials introduce new features, with polaron-related ideas emerging for uranium dioxide, gate dielectric oxides, Jahn-Teller systems, semiconducting polymers and biological systems. The phonon modes that initiate self-trapping can be quite different from the longitudinal optic modes usually assumed to dominate. Fourth, there are new phenomena, like possible magnetism in simple oxides, or with the evolution of short-lived polarons, like muons or excitons. The central idea remains that of a particle whose properties are modified by polarizing or deforming its host solid, sometimes profoundly. However, some of the simpler standard assumptions can give a limited, indeed misleading, description of real systems, with qualitative inconsistencies. We discuss representative cases for which theory and experiment can be compared in detail

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

    Science.gov (United States)

    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.

  15. Microfluidic PMMA interfaces for rectangular glass capillaries

    International Nuclear Information System (INIS)

    Evander, Mikael; Tenje, Maria

    2014-01-01

    We present the design and fabrication of a polymeric capillary fluidic interface fabricated by micro-milling. The design enables the use of glass capillaries with any kind of cross-section in complex microfluidic setups. We demonstrate two different designs of the interface; a double-inlet interface for hydrodynamic focusing and a capillary interface with integrated pneumatic valves. Both capillary interfaces are presented together with examples of practical applications. This communication shows the design optimization and presents details of the fabrication process. The capillary interface opens up for the use of complex microfluidic systems in single-use glass capillaries. They also enable simple fabrication of glass/polymer hybrid devices that can be beneficial in many research fields where a pure polymer chip negatively affects the device's performance, e.g. acoustofluidics. (technical note)

  16. Residual diesel measurement in sand columns after surfactant/alcohol washing

    International Nuclear Information System (INIS)

    Martel, R.; Gelinas, P.J.

    1996-01-01

    A new simple gravimetric technique has been designed to determine residual oil saturation of complex hydrocarbon mixtures (e.g., diesel) in sand column experiments because reliable methods are lacking. The He/N 2 technique is based on drying of sand columns by circulating helium gas to drag oil droplets in a cold trap (liquid nitrogen). With this technique, residual diesel measurement can be performed easily immediately after alcohol/surfactant washing and in the same lab. For high residual diesel content in Ottawa sand (25 to 30 g/kg), the technique is much more accurate (± 2% or 600 mg/kg) than the standard analytical methods for the determination of mineral oil and grease. The average relative error on partial diesel dissolution in sand column estimated after alcohol/surfactant flooding (residual saturation of 10 to 15 g/kg) is as low as 5%. The precision of the He/N 2 technique is adequate to compare relative efficiency of washing solutions when partial extraction of residual oil in Ottawa sand columns is performed. However, this technique is not adapted for determination of traces of oil in sediment or for environmental control of contaminated soils. Each diesel determination by the He/N 2 technique costs less than $8 in chemical products (helium and liquid nitrogen). A simple laboratory drying setup can be built for less than $400 which makes this technique valuable for diesel analyses when a large number of tests are required

  17. Capillary density and capillary-to-fibre ratio in vastus lateralis muscle of untrained and trained men.

    Science.gov (United States)

    Zoladz, J A; Semik, D; Zawadowska, B; Majerczak, J; Karasinski, J; Kolodziejski, L; Duda, K; Kilarski, W M

    2005-01-01

    Muscle fibre profile area (Af), volume density (Vv), capillary-to-fibre ratio (CF) and number of capillaries per fibre square millimetre (CD) were determined from needle biopsies of vastus lateralis of twenty-four male volunteers (mean +/- SD: age 25.4+/-5.8 years, height 178.6+/-5.5 cm, body mass 72.1+/-7.7 kg) of different training background. Seven subjects were untrained students (group A), nine were national and sub-national level endurance athletes (group B) with the background of 7.8+/-2.9 years of specialised training, and eight subjects were sprint-power athletes (group C) with 12.8+/-8.7 years of specialised training. Muscle biopsies of vastus lateralis were analysed histochemically for mATPase. Capillaries were visualized and counted using CD31 antibodies against endothelial cells. There were significant differences in the Vv of type I and type II muscle fibres in both trained groups, B (51.8%; 25.6%) and C (50.5%; 26.4%). However, in untrained group A that was treated as a reference group, the difference between Vv of type I and type II fibres was less prominent, nevertheless statistically significant (42.1%; 35.1%). There was also a significant difference in CF: 1.9 in group A and 2.1 in groups B and C. The number of capillaries per mm2 (CD) was 245 (group A), 308 (group B) and 325 (group C). Significant differences (Pski-jumping, volleyball, soccer and modern dance.

  18. Characteristics of trapped electrons and electron traps in single crystals

    International Nuclear Information System (INIS)

    Budzinski, E.E.; Potter, W.R.; Potienko, G.; Box, H.C.

    1979-01-01

    Two additional carbohydrates are reported whose crystal structures trap electrons intermolecularly in single crystals x irradiated at low temperature, namely sucrose and rhamnose. Five carbohydrate and polyhydroxy compounds are now known which exhibit this phenomenon. The following characteristics of the phenomenon were investigated: (1) the hyperfine couplings of the electron with protons of the polarized hydroxy groups forming the trap; (2) the distances between these protons and the trapped electron; (3) the spin density of the electron at the protons and (4) the relative stabilities of the electron trapped in various crystal structures

  19. Motion of guiding center drift atoms in the electric and magnetic field of a Penning trap

    International Nuclear Information System (INIS)

    Kuzmin, S.G.; O'Neil, T.M.

    2005-01-01

    The ApparaTus for High precision Experiment on Neutral Antimatter and antihydrogen TRAP collaborations have produced antihydrogen atoms by recombination in a cryogenic antiproton-positron plasma. This paper discusses the motion of the weakly bound atoms in the electric and magnetic field of the plasma and trap. The effective electric field in the moving frame of the atom polarizes the atom, and then gradients in the field exert a force on the atom. An approximate equation of motion for the atom center of mass is obtained by averaging over the rapid internal dynamics of the atom. The only remnant of the atom internal dynamics that enters this equation is the polarizability for the atom. This coefficient is evaluated for the weakly bound and strongly magnetized (guiding center drift) atoms understood to be produced in the antihydrogen experiments. Application of the approximate equation of motion shows that the atoms can be trapped radially in the large space charge field near the edge of the positron column. Also, an example is presented for which there is full three-dimensional trapping, not just radial trapping. Even untrapped atoms follow curved trajectories, and such trajectories are discussed for the important class of atoms that reach a field ionization diagnostic. Finally, the critical field for ionization is determined as an upper bound on the range of applicability of the theory

  20. Electro-capillary effects in capillary filling dynamics of electrorheological fluids.

    Science.gov (United States)

    Dhar, Jayabrata; Ghosh, Uddipta; Chakraborty, Suman

    2015-09-21

    The flow of electrorheological fluids is characterized by an apparent increase in viscosity manifested by the yield stress property of the fluid, which is a function of the applied electric field and the concentration of the suspended solute phase within the dielectric medium. This property of electrorheological fluids generally hinders flow through a capillary if the imposed shear stress is lower than the induced yield stress. This results in a plug-like zone in the flow profile, thus giving the fluid Bingham plastic properties. In the present work, we study such influences of the yield stress on the capillary filling dynamics of an electrorheological fluid by employing a rheologically consistent reduced order formalism. One important feature of the theoretical formalism is its ability to address the intricate interplay between the surface tension and viscous forces, both of which depend sensitively on the electric field. Our analysis reveals that the progress of the capillary front is hindered at an intermediate temporal regime, which is attributable to the increase of the span of the plug-zone across the channel width with time. With a preliminary understanding on the cessation of the capillary front advancement due to the yield stress property of the electrorheological fluids, we further strive to achieve a basic comparison with an experimental study made earlier. Reasonable agreements with the reported data support our theoretical framework. Comprehensive scaling analysis brings further insight to our reported observations over various temporal regimes.

  1. Capillary waves in slow motion

    International Nuclear Information System (INIS)

    Seydel, Tilo; Tolan, Metin; Press, Werner; Madsen, Anders; Gruebel, Gerhard

    2001-01-01

    Capillary wave dynamics on glycerol surfaces has been investigated by means of x-ray photon correlation spectroscopy performed at grazing angles. The measurements show that thermally activated capillary wave motion is slowed down exponentially when the sample is cooled below 273 K. This finding directly reflects the freezing of the surface waves. The wave-number dependence of the measured time constants is in quantitative agreement with theoretical predictions for overdamped capillary waves

  2. X-ray focusing using capillary arrays

    International Nuclear Information System (INIS)

    Nugent, K.A.; Chapman, H.N.

    1990-01-01

    A new form of X-ray focusing device based on glass capillary arrays is presented. Theoretical and experimental results for array of circular capillaries and theoretical and computational results for square hole capillaries are given. It is envisaged that devices such as these will find wide applications in X-ray optics as achromatic condensers and collimators. 3 refs., 4 figs

  3. Quantification of nucleotides by ICPMS: coupling of ICPMS with capillary electrophoresis or capillary HPLC

    International Nuclear Information System (INIS)

    Inagaki, K.; Fujii, S.; Takatsu, A.; Yarita, T.; Zhu, Y.; Chiba, K.

    2009-01-01

    Full text: Quantification of nucleotides in small volumes of biological samples has eagerly been demanded. A method using ICPMS coupled with capillary electrophoresis or capillary liquid chromatography is reported. A new interface system, which consists of a double tube nebulizer inserted with a fused silica capillary tube and a cylinder mini-chamber with a sheath gas inlet, was designed. Moreover, the surface conditions of the sampling and skimmer cones, and the introduction of H 2 gas into the plasma were found to significantly improve the signal/background ratio for phosphorus determination at m/z 31. (author)

  4. Micro-injector for capillary electrophoresis.

    Science.gov (United States)

    Sáiz, Jorge; Koenka, Israel Joel; García-Ruiz, Carmen; Müller, Beat; Chwalek, Thomas; Hauser, Peter C

    2015-08-01

    A novel micro-injector for capillary electrophoresis for the handling of samples with volumes down to as little as 300 nL was designed and built in our laboratory for analyses in which the available volume is a limitation. The sample is placed into a small cavity located directly in front of the separation capillary, and the injection is then carried out automatically by controlled pressurization of the chamber with compressed air. The system also allows automated flushing of the injection chamber as well as of the capillary. In a trial with a capillary electrophoresis system with contactless conductivity detector, employing a capillary of 25 μm diameter, the results showed good stability of migration times and peak areas. To illustrate the technique, the fast separation of five inorganic cations (Na(+) , K(+) , NH4 (+) , Ca(2+) , and Mg(2+) ) was set up. This could be achieved in less than 3 min, with good limits of detection (10 μM) and linear ranges (between about 10 and 1000 μM). The system was demonstrated for the determination of the inorganic cations in porewater samples of a lake sediment core. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Fast and repetitive in-capillary production of [{sup 18}F]FDG

    Energy Technology Data Exchange (ETDEWEB)

    Wester, Hans-Juergen; Schoultz, Bent Wilhelm; Hultsch, Christina; Henriksen, Gjermund [Technische Universitaet Muenchen, Department of Nuclear Medicine, Klinikum rechts der Isar, Munich (Germany)

    2009-04-15

    The increasing demand for radiopharmaceuticals to be provided reproducibly and flexibly with high frequency for clinical application and animal imaging would be better met by improved or even new strategies for automated tracer production. Radiosynthesis in microfluidic systems, i.e. narrow tubing with a diameter of approximately 50-500 {mu}m, holds promise for providing the means for repetitive multidose and multitracer production. In this study, the performance of a conceptually simple microfluidic device integrated into a fully automated synthesis procedure for in-capillary radiosynthesis (ICR) of clinical grade [{sup 18}F]FDG was evaluated. The instrumental set-up consisted of pumps for reagent and solvent delivery into small mixing chambers, {mu}-fluidic capillaries, in-process radioactivity monitoring, solid-phase extraction and on-column deprotection of the {sup 18}F-labelled intermediate followed by on-line formulation of [{sup 18}F]FDG. In-capillary{sup 18}F-fluorination of 2.1 {mu}mol 1,3,4,6-tetra-O-acetyl-2-O-trifluoromethanesulphonyl-beta-d-mannopyranose (TATM; precursor for [{sup 18}F]FDG) in acetonitrile (MeCN) at a flow rate of 0.3 ml/min within 40 s and subsequent on-line hydrolysis of the intermediate by treatment with 0.3 M NaOH for 1 min at 40 C resulted in a radiochemical yield of 88 {+-} 4% within <7 min. Reproducibility, robustness and suitability as a fast and efficient radiopharmaceutical research tool for {sup 18}F-fluorination was demonstrated by eight independent, sequentially performed ICRs which provided identical tracer quality (radiochemical purity >97%, MeCN <5 {mu}g/ml) and similar absolute yields (approximately 1.4 GBq). The described ICR process is a simple and efficient alternative to classic radiotracer production systems and provides a comparatively cheap instrumental methodology for the repetitive production of [{sup 18}F]FDG with remarkably high efficiency and high yield under fully automated conditions. Although the results

  6. Capillary condenser/evaporator

    Science.gov (United States)

    Valenzuela, Javier A. (Inventor)

    2010-01-01

    A heat transfer device is disclosed for transferring heat to or from a fluid that is undergoing a phase change. The heat transfer device includes a liquid-vapor manifold in fluid communication with a capillary structure thermally connected to a heat transfer interface, all of which are disposed in a housing to contain the vapor. The liquid-vapor manifold transports liquid in a first direction and conducts vapor in a second, opposite direction. The manifold provides a distributed supply of fluid (vapor or liquid) over the surface of the capillary structure. In one embodiment, the manifold has a fractal structure including one or more layers, each layer having one or more conduits for transporting liquid and one or more openings for conducting vapor. Adjacent layers have an increasing number of openings with decreasing area, and an increasing number of conduits with decreasing cross-sectional area, moving in a direction toward the capillary structure.

  7. Design of Capillary Flows with Spatially Graded Porous Films

    Science.gov (United States)

    Joung, Young Soo; Figliuzzi, Bruno Michel; Buie, Cullen

    2013-11-01

    We have developed a new capillary tube model, consisting of multi-layered capillary tubes oriented in the direction of flow, to predict capillary speeds on spatially graded porous films. Capillary flows through thin porous media have been widely utilized for small size liquid transport systems. However, for most media it is challenging to realize arbitrary shapes and spatially functionalized micro-structures with variable flow properties. Therefore, conventional media can only be used for capillary flows obeying Washburn's equation and the modifications thereof. Given this background, we recently developed a method called breakdown anodization (BDA) to produce highly wetting porous films. The resulting surfaces show nearly zero contact angles and fast water spreading speed. Furthermore, capillary pressure and spreading diffusivity can be expressed as functions of capillary height when customized electric fields are used in BDA. From the capillary tube model, we derived a general capillary flow equation of motion in terms of capillary pressure and spreading diffusivity. The theoretical model shows good agreement with experimental capillary flows. The study will provide novel design methodologies for paper-based microfluidic devices.

  8. Test procedure for calibration, grooming and alignment of the LDUA Purge Air Supply System

    International Nuclear Information System (INIS)

    Potter, J.D.

    1995-01-01

    The Light Duty Utility Arm (LDUA) is a remotely operated manipulator used to enter into underground waste tanks through one of the tank risers. National Electric Code requirements mandate that the in-tank portions of the LDUA be maintained at a positive pressure for entrance into a flammable atmosphere. The LDUA Purge Air Supply System (PASS) is a small, portable air compressor, which provides a constant low flow of instrument grade air for this purpose. This procedure is used to assure that the instrumentation and equipment comprising the PASS is properly adjusted in order to achieve its intended functions successfully

  9. Modeling Stone Columns.

    Science.gov (United States)

    Castro, Jorge

    2017-07-11

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

  10. Ion guiding in macro-size insulating capillaries: straight, tapered, and curved shapes

    Science.gov (United States)

    Kojima, Takao M.

    2018-02-01

    When keV energy ions are injected into a tilted insulating capillary, a certain fraction of the injected ions are transported through the tilt angle of the capillary. This ion guiding phenomenon is considered to be caused by a self-organizing charge distribution, where the inner wall of the capillary becomes charged by initial incoming ions. The charge distribution, which is formed, can guide following ions toward the exit of the capillary. Since the initial discovery of this effect, studies of ion guiding by insulating capillaries have been extended to various materials, and different sizes and shapes of capillaries. In recent years, some investigations of the guiding effect of macro-size curved capillaries have also been reported. In this review, relevant studies in a history of ion guiding in curved capillaries are discussed and future directions in this field are considered.

  11. Proper Use of Capillary Number in Chemical Flooding

    Directory of Open Access Journals (Sweden)

    Hu Guo

    2017-01-01

    Full Text Available Capillary number theory is very important for chemical flooding enhanced oil recovery. The difference between microscopic capillary number and the microscopic one is easy to confuse. After decades of development, great progress has been made in capillary number theory and it has important but sometimes incorrect application in EOR. The capillary number theory was based on capillary tube bundles and Darcy’s law hypothesis, and this should always be kept in mind when used in chemical flooding EOR. The flow in low permeability porous media often shows obvious non-Darcy effects, which is beyond Darcy’s law. Experiments data from ASP flooding and SP flooding showed that remaining oil saturation was not always decreasing as capillary number kept on increasing. Relative permeability was proved function of capillary number; its rate dependence was affected by capillary end effects. The mobility control should be given priority rather than lowering IFT. The displacement efficiency was not increased as displacement velocity increased as expected in heavy oil chemical flooding. Largest capillary number does not always make highest recovery in chemical flooding in heterogeneous reservoir. Misuse of CDC in EOR included the ignorance of mobility ratio, Darcy linear flow hypothesis, difference between microscopic capillary number and the microscopic one, and heterogeneity caused flow regime alteration. Displacement of continuous oil or remobilization of discontinuous oil was quite different.

  12. Coral mucus functions as an energy carrier and particle trap in the reef ecosystem

    DEFF Research Database (Denmark)

    Wild, C.; Huettel, M.; Klueter, A.

    2004-01-01

    Zooxanthellae, endosymbiotic algae of reef-building corals, substantially contribute to the high gross primary production of coral reefs(1), but corals exude up to half of the carbon assimilated by their zooxanthellae as mucus(2,3). Here we show that released coral mucus efficiently traps organic...... matter from the water column and rapidly carries energy and nutrients to the reef lagoon sediment, which acts as a biocatalytic mineralizing filter. In the Great Barrier Reef, the dominant genus of hard corals, Acropora, exudes up to 4.8 litres of mucus per square metre of reef area per day. Between 56......% and 80% of this mucus dissolves in the reef water, which is filtered through the lagoon sands. Here, coral mucus is degraded at a turnover rate of at least 7% per hour. Detached undissolved mucus traps suspended particles, increasing its initial organic carbon and nitrogen content by three orders...

  13. Post column derivatisation analyses review. Is post-column derivatisation incompatible with modern HPLC columns?

    Science.gov (United States)

    Jones, Andrew; Pravadali-Cekic, Sercan; Dennis, Gary R; Shalliker, R Andrew

    2015-08-19

    Post Column derivatisation (PCD) coupled with high performance liquid chromatography or ultra-high performance liquid chromatography is a powerful tool in the modern analytical laboratory, or at least it should be. One drawback with PCD techniques is the extra post-column dead volume due to reaction coils used to enable adequate reaction time and the mixing of reagents which causes peak broadening, hence a loss of separation power. This loss of efficiency is counter-productive to modern HPLC technologies, -such as UHPLC. We reviewed 87 PCD methods published from 2009 to 2014. We restricted our review to methods published between 2009 and 2014, because we were interested in the uptake of PCD methods in UHPLC environments. Our review focused on a range of system parameters including: column dimensions, stationary phase and particle size, as well as the geometry of the reaction loop. The most commonly used column in the methods investigated was not in fact a modern UHPLC version with sub-2-micron, (or even sub-3-micron) particles, but rather, work-house columns, such as, 250 × 4.6 mm i.d. columns packed with 5 μm C18 particles. Reaction loops were varied, even within the same type of analysis, but the majority of methods employed loop systems with volumes greater than 500 μL. A second part of this review illustrated briefly the effect of dead volume on column performance. The experiment evaluated the change in resolution and separation efficiency of some weak to moderately retained solutes on a 250 × 4.6 mm i.d. column packed with 5 μm particles. The data showed that reaction loops beyond 100 μL resulted in a very serious loss of performance. Our study concluded that practitioners of PCD methods largely avoid the use of UHPLC-type column formats, so yes, very much, PCD is incompatible with the modern HPLC column. Copyright © 2015. Published by Elsevier B.V.

  14. Highly efficient pulsed power supply system with a two-stage LC generator and a step-up transformer for fast capillary discharge soft x-ray laser at shorter wavelength

    International Nuclear Information System (INIS)

    Sakai, Yusuke; Takahashi, Shnsuke; Komatsu, Takanori; Song, Inho; Watanabe, Masato; Hotta, Eiki

    2010-01-01

    Highly efficient and compact pulsed power supply system for a capillary discharge soft x-ray laser (SXRL) has been developed. The system consists of a 2.2 μF two-stage LC inversion generator, a 2:54 step-up transformer, a 3 nF water capacitor, and a discharge section with a few tens of centimeter length capillary. Adoption of the pulsed transformer in combination with the LC inversion generator enables us to use only one gap switch in the circuit for charging the water capacitor up to about 0.5 MV. Furthermore, step-up ratio of a water capacitor voltage to a LC inversion generator initial charging voltage is about 40 with energy transfer efficiency of about 50%. It also leads to good reproducibility of a capillary discharge which is necessary for lasing a SXRL stably. For the study of the possibility of lasing a SXRL at shorter wavelength in a small laboratory scale, high-density and high-temperature plasma column suitable for the laser can be generated relatively easily with this system.

  15. Transmission of fast highly charged ions through straight and tapered glass capillaries

    International Nuclear Information System (INIS)

    Ayyad, Asma M; Keerthisinghe, D; Kayani, A; Tanis, J A; Dassanayake, B S; Ikeda, T

    2013-01-01

    The transmission of 1 and 3 MeV protons through a borosilicate straight glass capillary and a tapered glass capillary was investigated. The straight capillary had a diameter of ∼0.18 mm and a length of ∼14.4 mm, while the tapered capillary had an inlet diameter of ∼0.71 mm, an outlet diameter of ∼0.10 mm and a length of ∼28 mm. The results show that the 1 and 3 MeV protons traverse through both samples without energy loss, while the tapered capillary showed better transmission than the straight capillary. (paper)

  16. Study of glow discharge positive column with cloud of disperse particles

    International Nuclear Information System (INIS)

    Polyakov, D.N.; Shumova, V.V.; Vasilyak, L.M.; Fortov, V.E.

    2011-01-01

    The study aims to describe plasma parameters changes induced by clouds of disperse micron size particles. Dust clouds were formed in the positive column of glow discharge in air at pressure 0.1-0.6 torr and current 0.1-3 mA. The simultaneous registration of discharge voltage and dust cloud parameters was carried out. Experimental results were simulated using diffusion model. The dust cloud is shown to smooth the radial electron concentration profile, increase electric field strength and electron temperature and stabilize the discharge. The cloud is demonstrated to be a trap for positive ions without increase of discharge current. -- Highlights: → 25% increase of longitudinal electric field strength in discharge with dust cloud. → The smoothing effect of dust cloud on radial electron and ion concentration profiles. → Dust cloud as a trap for positive ions without increase of discharge current. → Increase of electron temperature in discharge with dust cloud. → Increase of discharge stability in presence of dust cloud.

  17. Sheathless interface for coupling capillary electrophoresis with mass spectrometry

    Science.gov (United States)

    Wang, Chenchen; Tang, Keqi; Smith, Richard D.

    2014-06-17

    A sheathless interface for coupling capillary electrophoresis (CE) with mass spectrometry is disclosed. The sheathless interface includes a separation capillary for performing CE separation and an emitter capillary for electrospray ionization. A portion of the emitter capillary is porous or, alternatively, is coated to form an electrically conductive surface. A section of the emitter capillary is disposed within the separation capillary, forming a joint. A metal tube, containing a conductive liquid, encloses the joint.

  18. Speciation—targets, analytical solutions and markets

    Science.gov (United States)

    Łobiński, Ryszard

    1998-02-01

    An analysis of speciation-relevant issues leads to the conclusion that, despite the rapidly increasing number of reports, the field has reached a level of virtual stagnation in terms of research originality and market perspectives. A breakthrough is in sight but requires an advanced interdisciplinary collaboration of chemists-analysts with clinicians, ecotoxicologists and nutricionists aimed at the definition of metal (metalloid)-dependent problems relevant to human health. The feedback from analytical chemists will be stimulated by a wider availability of efficient HPLC (CZE)-inductively coupled plasma mass spectrometry (ICP MS) interfaces, chromatographic software for ICP AES and MS and sensitive on-line methods for compound identification (electrospray MS/MS). The maturity of purge and trap thermal desorption techniques and capillary GC chromatography is likely to be reflected by an increasing number of commercial dedicated systems for small molecules containing Hg, Pb, Sn and metalloids. The pre-requisite of success for such systems is the integration of a sample preparation step (based on focused low-power microwave technology) into the marketed set-up.

  19. Development of a Capillary-driven, Microfluidic, Nucleic Acid Biosensor

    Directory of Open Access Journals (Sweden)

    Fei HE

    2011-12-01

    Full Text Available An ideal point-of-care device would incorporate the simplicity and reliability of a lateral flow assay with a microfluidic device. Our system consists of self-priming microfluidics with sealed conjugate pads of reagent delivery and an absorbent pad for additional fluid draw. Using poly (methyl methacrylate (PMMA as a substrate, we have developed a single-step surface modification method which allows strong capillary flow within a sealed microchannel. Conjugate pads within the device held trapped complex consisting of the magnetic beads and nucleic-acid-probe-conjugated horseradish peroxidase (HRP. Magnetic beads were released when sample entered the chamber and hybridized with the complex. The complex was immobilized over a magnet while a luminol co-reactant stream containing H2O2 was merged with the channel. A plate reader was able to quantify the chemiluminescence signal. This new format of biosensor will allow for a smaller and more sensitive biosensor, as well as commercial-scale manufacturing and low materials cost.

  20. Reliability of widefield capillary microscopy to measure nailfold capillary density in systemic sclerosis.

    Science.gov (United States)

    Hudson, M; Masetto, A; Steele, R; Arthurs, E; Baron, M

    2010-01-01

    To determine intra- and inter-observer reliability of widefield microscopy to measure nailfold capillary density in patients with systemic sclerosis (SSc). Five SSc patients were examined with a STEMV-8 Zeiss biomicroscope with 50x magnification. The nailfold of the second, third, fourth and fifth fingers of both hands of each patient were photographed twice by each of two observers, once in the morning and again in the afternoon (total of 32 pictures). Two raters reviewed the photographs to produce capillary density readings. Intra- and inter-rater reliability of the readings were computed using intra-class correlations (ICC). Additional analyses were undertaken to determine the impact of other sources of variability in the data, namely patient, finger, technician and time. Intra-and inter-rater reliability were substantial (ICC 0.72-0.84) when raters were reading the same photographs or photographs taken at the same time of day. Agreement was only fair between morning and afternoon density readings (ICC 0.30-0.37). Patients, individual fingers and technician accounted for a large part of the variability in the data (combined variance component of 7.69 out of the total 12.23). The coefficient of variation of widefield microscopy was 24%. Although intra- and inter-rater reliability of nailfold capillary density measurements using widefield microscopy are good, proper standardisation of the conditions under which capillaroscopy is done and better imaging of nailfold capillary abnormalities should be considered if nailfold capillary density is to be used as an outcome measure in multi-centre clinical trials in SSc.