• Title/Summary/Keyword: Packing phase

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Full validation of high-throughput bioanalytical method for the new drug in plasma by LC-MS/MS and its applicability to toxicokinetic analysis

  • Han, Sang-Beom
    • Proceedings of the Korean Society of Toxicology Conference
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    • 2006.11a
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    • pp.65-74
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    • 2006
  • Modem drug discovery requires rapid pharmacokinetic evaluation of chemically diverse compounds for early candidate selection. This demands the development of analytical methods that offer high-throughput of samples. Naturally, liquid chromatography / tandem mass spectrometry (LC-MS/MS) is choice of the analytical method because of its superior sensitivity and selectivity. As a result of the short analysis time(typically 3-5min) by LC-MS/MS, sample preparation has become the rate- determining step in the whole analytical cycle. Consequently tremendous efforts are being made to speed up and automate this step. In a typical automated 96-well SPE(solid-phase extraction) procedure, plasma samples are transferred to the 96-well SPE plate, internal standard and aqueous buffer solutions are added and then vacuum is applied using the robotic liquid handling system. It takes only 20-90 min to process 96 samples by automated SPE and the analyst is physically occupied for only approximately 10 min. Recently, the ultra-high flow rate liquid chromatography (turbulent-flow chromatography)has sparked a huge interest for rapid and direct quantitation of drugs in plasma. There is no sample preparation except for sample aliquotting, internal standard addition and centrifugation. This type of analysis is achieved by using a small diameter column with a large particle size(30-5O ${\mu}$m) and a high flow rate, typically between 3-5 ml/min. Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of pcrous silica. The main advantage of such a network is decreased backpressure due to macropores (2 ${\mu}$m) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The reduction of particle diameter in HPLC results in increased column efficiency. use of small particles (<2 urn), however, requires p.essu.es beyond the traditional 6,000 psi of conventional pumping devices. Instrumental development in recent years has resulted in pumping devices capable of handling the requirements of columns packed with small particles. The staggered parallel HPLC system consists of four fully independent binary HPLC pumps, a modified auto sampler, and a series of switching and selector valves all controlled by a single computer program. The system improves sample throughput without sacrificing chromatographic separation or data quality. Sample throughput can be increased nearly four-fold without requiring significant changes in current analytical procedures. The process of Bioanalytical Method Validation is required by the FDA to assess and verify the performance of a chronlatographic method prior to its application in sample analysis. The validation should address the selectivity, linearity, accuracy, precision and stability of the method. This presentation will provide all overview of the work required to accomplish a full validation and show how a chromatographic method is suitable for toxirokinetic sample analysis. A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method developed to quantitate drug levels in dog plasma will be used as an example of tile process.

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Synthesis and Structural Analysis of Binary Alloy ($MoRu_3$, $MoRh_3$) (이성분계 금속합금($MoRu_3$, $MoRh_3$)의 합성 및 구조분석)

  • Park, Yong Joon;Lee, Jong-Gyu;Kim, Jong Goo;Kim, Jung Suk;Jee, Kwang-Yong
    • Analytical Science and Technology
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    • v.11 no.3
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    • pp.189-193
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    • 1998
  • Binary alloys, $MoRu_3$ and $MoRh_3$, have been prepared using arc melting furnace. Mo and the noble metals Ru and Rh are the constituents of metallic insoluble residues, which were found in the early days of the post-irradiation studies on uranium oxide fuels. Detailed structural informations about these alloys have not been reported on JCPDS files of ICDD (International Centre for Diffraction Data). The results of X-ray diffraction study showed that the alloy was crystallized in hexagonal close-packing, well known as ${\varepsilon}$-phase. The X-ray diffraction patterns of these alloys matched well to that of $WRh_3$ with $P6_3/mmc$ of space group. The lattice parameters, a and c, were calculated using the least squares extrapolation. It was found from X-ray photoelectron spectroscopic measurements that Mo on the surface of the alloy was oxidized to Mo(6+), which could be removed by sputtering with Ar ions for approximately 15 minutes. The changes in binding energy of Mo, Ru, and Rh on the surface of the alloy were not observed. Magnetic susceptibility measurements resulted in the typical Pauli-paramagnetic behavior in the temperature range of 2 to 300 K.

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A Study of EPMA Analysis for Nitric Acid Insoluble Alloys (질산불용성 합금의 EPMA분석)

  • Park, Soon-Dal;Park, Yong-Joon;Kim, Jong-Goo;Son, Se-Chul;Joe, Kih-Soo
    • Analytical Science and Technology
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    • v.11 no.6
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    • pp.485-494
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    • 1998
  • Ternary and quaternary alloys composed of Mo-Ru-Rh-Pd were prepared and their crystal structure and quantitative chemical compositions were analysed by XRD, WDX, EDX and ICP/AES. The results of X-ray diffraction studies showed that the alloys were crystallized in hexagonal close packing, well known as ${\varepsilon}$-phase with $P6_3/mmc$ of space group. The optimum accelerating voltage for Zr~Cd(40~48) analyzed by EPMA using PET crystal was found to be 15 kV and the linear regression coefficient(R) of atomic number and X-ray intensity was approximately 0.998 without Tc standard specimen. The WDX results of alloys of Mo and Pd by linear regression equations were detected to be 0.1% lower compared to WDX analysis results using standard specimen, while Ru, Rh were detected 3% higher. These alloys were completely dissolved in mixed acid of 12.5 mL HCl and 1 mL $HNO_3$, at $220^{\circ}C$ for 22 hours using autoclave with PTFE vessel. There was no reprecipitating phenomnon when diluted 100 times with 1N-HCl. The results of ICP/AES analysis deviated less than 4% comparing with those of normal WDX analysis.

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A Study on Drying Kinetics of Low Rank Coal(Indonesia-IBC) through the Fixed-Bed Reactor Experiments (저등급석탄(低等級石炭)(인도네시아 IBC)의 고정층(固定層) 반응기(反應器) 실험(實驗)을 통한 건조(乾操) 반응속도론(反應速度論) 연구(硏究))

  • Kang, Tae-Jin;Jeon, Do-Man;Jeon, Young-Sin;Kang, Suk-Hwan;Lee, Si-Hyun;Kim, Sang-Do;Kim, Hyung-Taek
    • Resources Recycling
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    • v.19 no.6
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    • pp.43-50
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    • 2010
  • The crisis of energy gives rise to the growing concerns over continuing uncertainty in the energy market. Under these circumstances, there are also increasing interests on coals. In particular, Low Rank Coal (LRC) is receiving gradual attentions from green industry. But due to is high moisture content range from 30 - 60%, drying process has to be preceded before being utilized as power plant. In this study drying kinetics of LRC is induced by using a fixed-bed reactor. The drying kinetics was evaluated in from of the particle size, the inlet gas temperature, the drying time, the gas velocity, and the LID ratio. The consideration of the reynold's number was taken for correction of gas velocity, particle size and LID was taken for correction of reactor diameter, packing height of coal. As being seen as characteristic of drying coal, it can be found that fixed-bed reactor can contributed to active drying of free water. In this sense, it could be considered that phase boundary reaction is appropriate mechanism.

Recent Progress in Air-Conditioning and Refrigeration Research : A Review of Papers Published in the Korean Journal of Air-Conditioning and Refrigeration Engineering in 2016 (설비공학 분야의 최근 연구 동향 : 2016년 학회지 논문에 대한 종합적 고찰)

  • Lee, Dae-Young;Kim, Sa Ryang;Kim, Hyun-Jung;Kim, Dong-Seon;Park, Jun-Seok;Ihm, Pyeong Chan
    • Korean Journal of Air-Conditioning and Refrigeration Engineering
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    • v.29 no.6
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    • pp.327-340
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    • 2017
  • This article reviews the papers published in the Korean Journal of Air-Conditioning and Refrigeration Engineering during 2016. It is intended to understand the status of current research in the areas of heating, cooling, ventilation, sanitation, and indoor environments of buildings and plant facilities. Conclusions are as follows. (1) The research works on the thermal and fluid engineering have been reviewed as groups of flow, heat and mass transfer, the reduction of pollutant exhaust gas, cooling and heating, the renewable energy system and the flow around buildings. CFD schemes were used more for all research areas. (2) Research works on heat transfer area have been reviewed in the categories of heat transfer characteristics, pool boiling and condensing heat transfer and industrial heat exchangers. Researches on heat transfer characteristics included the results of the long-term performance variation of the plate-type enthalpy exchange element made of paper, design optimization of an extruded-type cooling structure for reducing the weight of LED street lights, and hot plate welding of thermoplastic elastomer packing. In the area of pool boiling and condensing, the heat transfer characteristics of a finned-tube heat exchanger in a PCM (phase change material) thermal energy storage system, influence of flow boiling heat transfer on fouling phenomenon in nanofluids, and PCM at the simultaneous charging and discharging condition were studied. In the area of industrial heat exchangers, one-dimensional flow network model and porous-media model, and R245fa in a plate-shell heat exchanger were studied. (3) Various studies were published in the categories of refrigeration cycle, alternative refrigeration/energy system, system control. In the refrigeration cycle category, subjects include mobile cold storage heat exchanger, compressor reliability, indirect refrigeration system with $CO_2$ as secondary fluid, heat pump for fuel-cell vehicle, heat recovery from hybrid drier and heat exchangers with two-port and flat tubes. In the alternative refrigeration/energy system category, subjects include membrane module for dehumidification refrigeration, desiccant-assisted low-temperature drying, regenerative evaporative cooler and ejector-assisted multi-stage evaporation. In the system control category, subjects include multi-refrigeration system control, emergency cooling of data center and variable-speed compressor control. (4) In building mechanical system research fields, fifteenth studies were reported for achieving effective design of the mechanical systems, and also for maximizing the energy efficiency of buildings. The topics of the studies included energy performance, HVAC system, ventilation, renewable energies, etc. Proposed designs, performance tests using numerical methods and experiments provide useful information and key data which could be help for improving the energy efficiency of the buildings. (5) The field of architectural environment was mostly focused on indoor environment and building energy. The main researches of indoor environment were related to the analyses of indoor thermal environments controlled by portable cooler, the effects of outdoor wind pressure in airflow at high-rise buildings, window air tightness related to the filling piece shapes, stack effect in core type's office building and the development of a movable drawer-type light shelf with adjustable depth of the reflector. The subjects of building energy were worked on the energy consumption analysis in office building, the prediction of exit air temperature of horizontal geothermal heat exchanger, LS-SVM based modeling of hot water supply load for district heating system, the energy saving effect of ERV system using night purge control method and the effect of strengthened insulation level to the building heating and cooling load.

Perfluoropolymer Membranes of Tetrafluoroethylene and 2,2,4Trifluofo- 5Trifluorometoxy- 1,3Dioxole.

  • Arcella, V.;Colaianna, P.;Brinati, G.;Gordano, A.;Clarizia, G.;Tocci, E.;Drioli, E.
    • Proceedings of the Membrane Society of Korea Conference
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    • 1999.07a
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    • pp.39-42
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    • 1999
  • Perfluoropolymers represent the ultimate resistance to hostile chemical environments and high service temperature, attributed to the presence of fluorine in the polymer backbone, i.e. to the high bond energy of C-F and C-C bonds of fluorocarbons. Copolymers of Tetrafluoroethylene (TEE) and 2, 2, 4Trifluoro-5Trifluorometoxy- 1, 3Dioxole (TTD), commercially known as HYFLON AD, are amorphous perfluoropolymers with glass transition temperature (Tg)higher than room temperature, showing a thermal decomposition temperature exceeding 40$0^{\circ}C$. These polymer systems are highly soluble in fluorinated solvents, with low solution viscosities. This property allows the preparation of self-supported and composite membranes with desired membrane thickness. Symmetric and asymmetric perfluoropolymer membranes, made with HYFLON AD, have been prepared and evaluated. Porous and not porous symmetric membranes have been obtained by solvent evaporation with various processing conditions. Asymmetric membranes have been prepared by th wet phase inversion method. Measure of contact angle to distilled water have been carried out. Figure 1 compares experimental results with those of other commercial membranes. Contact angles of about 120$^{\circ}$for our amorphous perfluoropolymer membranes demonstrate that they posses a high hydrophobic character. Measure of contact angles to hexandecane have been also carried out to evaluate the organophobic character. Rsults are reported in Figure 2. The observed strong organophobicity leads to excellent fouling resistance and inertness. Porous membranes with pore size between 30 and 80 nanometers have shown no permeation to water at pressures as high as 10 bars. However high permeation to gases, such as O2, N2 and CO2, and no selectivities were observed. Considering the porous structure of the membrane, this behavior was expected. In consideration of the above properties, possible useful uses in th field of gas- liquid separations are envisaged for these membranes. A particularly promising application is in the field of membrane contactors, equipments in which membranes are used to improve mass transfer coefficients in respect to traditional extraction and absorption processes. Gas permeation properties have been evaluated for asymmetric membranes and composite symmetric ones. Experimental permselectivity values, obtained at different pressure differences, to various single gases are reported in Tab. 1, 2 and 3. Experimental data have been compared with literature data obtained with membranes made with different amorphous perfluoropolymer systems, such as copolymers of Perfluoro2, 2dimethyl dioxole (PDD) and Tetrafluorethylene, commercialized by the Du Pont Company with the trade name of Teflon AF. An interesting linear relationship between permeability and the glass transition temperature of the polymer constituting the membrane has been observed. Results are descussed in terms of polymer chain structure, which affects the presence of voids at molecular scale and their size distribution. Molecular Dyanmics studies are in progress in order to support the understanding of these results. A modified Theodoru- Suter method provided by the Amorphous Cell module of InsightII/Discover was used to determine the chain packing. A completely amorphous polymer box of about 3.5 nm was considered. Last but not least the use of amorphous perfluoropolymer membranes appears to be ideal when separation processes have to be performed in hostile environments, i.e. high temperatures and aggressive non-aqueous media, such as chemicals and solvents. In these cases Hyflon AD membranes can exploit the outstanding resistance of perfluoropolymers.

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