• Title/Summary/Keyword: vacuum time

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The Corrosion Behavior of Hydrogen-Charged Zircaloy-4 Alloys (수소 장입된 Zircaloy-4 합금에서의 부식거동)

  • Kim, Seon-Jae;Kim, Gyeong-Ho;Baek, Jong-Hyeok;Choe, Byeong-Gwon;Jeong, Yo-Hwan
    • Korean Journal of Materials Research
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    • v.8 no.3
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    • pp.268-273
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    • 1998
  • Standard Zircaloy-4 sheets, charged with 230-250ppm hydrogen by the gas-charging method and homogenized at $400^{\circ}C$ for 72hrs in a vacuum, were corroded in pure water and aqueous LiOH solutions using static autoclaves at $350^{\circ}C$. Their corrosion behaviors were characterized by measuring their weight gains with the corrosion time and observing their microstructures using an optical microscope and a scanning electron microscope. The elemental depth profiles for hydrogen and lithium were measured using a secondary ion mass spectrometry(S1MS) to confirm their distributions at the oxidelmetal interface. The normal Zircaloy-4 specimens corroded abruptly and heavily at the concentration of Li ions more than 30ppm in the aqueous solution. This is due to accelerations by the rapid oxidation of many Zr- hydrides formed by the large amount of absorbed hydrogen, resulting from the increased substitution of $Li^{+}$ ions with $Zr^{4+}$-sites in the oxide as the Li ion concentration increased. The specimens that had been charged with amounts of hydrogen greater than its solubility corroded early with a more rapid acceleration than normal specimens, regardless of the corrosion solutions. At longer corrosion times. however, normal specimens showed a rather accelerated corrosion rate compared to the hydrogen-charged specimens. These slower corrosion rates of the hydrogen-charged specimens at the longer corrosion times would be due to the pre-existent Zr-hydride in the matrix, which causes the hydrogen pick- up into the specimen to be depressed, when the oxide with an appropriate thickness formed.

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Desorption of organic Compounds from the Simulated Soils by Soil Vapor Extraction (인공토양으로부터 토양증기추출법에 의한 유기화합물의 탈착 현상에 관한 실험 연구)

  • 이병환;이종협
    • Journal of Korea Soil Environment Society
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    • v.3 no.2
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    • pp.101-114
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    • 1998
  • Soil vapor extraction (SVE) is known to be an effective process to remove the contaminants from the soils by enhancing the vaporization of organic compounds using forced vapor flows or applying vacuum through soils. Experiments are carried out to investigate the effects of the organic contaminants, types of soils, and water contents on the removal efficiency with operating time. In the study, simulated soils include the glass bead which has no micropore, sand and molecular sieve which has a large volume of micropores. As model organic pollutants, toluene, methyl ethyl ketone, and trichloroethylene are selected. Desorption experiments are conducted by flowing nitrogen gas. Under the experimental conditions, it is found that there are linear relationships between logarithm of removal efficiency and logarithm of number of pore volumes. The number of pore volumes are defined as the total amount of air flow through the soil column divided by the pore volume of soil column. For three organic compounds studied, the removal rate is slow for no water content, while the number of pore volumes for removal of organic compounds are notably reduced for water contents up to 37%. For the removal of dense organic compound, such as trichloroethylene, a large number of pore volumes are needed. Also, the effects of the characteristics of simulated soils on the removal efficiency of organic compounds are studied. After the characterization of soil surface, porosity of soil columns and types of contaminants, the results could provide a basis for the design of SVE process.

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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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Preservation of Fried Fish Meat Paste by Irradiation (감마선 조사에 의한 튀김어묵의 품질보존)

  • Cho, Han-Ok;Kwon, Joong-Ho;Byun, Myung-Woo;Lee, Mi-Kyung
    • Korean Journal of Food Science and Technology
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    • v.17 no.6
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    • pp.474-481
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    • 1985
  • Radurization effects on fried fish meat paste with Co-60 gamma irradiation at 0-5 kGy and physicochemical aspects of the stored samples at low ($3{\pm}1^{\circ}C$, LT) and room ($10-20^{\circ}C$, RT) temperatures were investigated. The initial microbial loads of the samples were $2.2{\times}10^3/g$ in total bacterial count, $2.8{\times}10^2/g$ in yeasts & molds, and $1.0{\times}10^2/g$ in coliform group, respectively. An irradiation dose of more than 3 kGy was shown to be effective for the radurization of stored samples and there is no apparent difference between air and vacuum packaging groups. The chemical components related to the quality underwent similar changes in the nonirradiated and irradiated groups; however, as the storage time was prolonged the quality of nonirradiated samples rapidly deteriorated. Textural parameters of the samples were little affected by the applied doses, and sensory evaluations showed that 3 kGy irradiation was the optimum dose level to extend the shelf-life of fried fish meat paste up to 2 times at RT and 3 to 4 times at LT, respectively compared with the nonirradiated control.

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Effect of Deodorizing Conditions on Formation of trans-Fatty Acids of Soybean Oil (대두유의 탈취과정에서 생성되는 trans 지방산의 정량)

  • Park, Choul-Soo;Yoon, Kwang-Ro
    • Korean Journal of Food Science and Technology
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    • v.30 no.1
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    • pp.6-12
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    • 1998
  • Degummed and bleached soybean oil was deodorized at a temperature range of $220{\sim}280^{\circ}C$ under the vacuum (4-5 torr) for 1 or 2 hrs. Gas chromatography with SP-2560 100 m capillary column was used to separate and quantitate fatty acid methyl esters and their isomers. Fatty acids were identified by comparing retention time with standards and GC-MS spectrum. The isomers of linoleic acid and linolenic acid in deodorized soybean oils were identified to be $C_{18:2}\;{\Delta}9-cis,\;{\Delta}12-trans,\;C_{18:2}\;{\Delta}9-trans,\;{\Delta}12-cis,\;C_{18:2}\;{\Delta}9-cis,\;{\Delta}12-cis,\;C_{18:3}\;{\Delta}9-cis,\;{\Delta}12-cis,\;{\Delta}15-trans,\;C_{18:3}\;{\Delta}9-trans,\;{\Delta}12-cis,\;{\Delta}15-cis,\;C_{18:3}\;{\Delta}9-cis,\;{\Delta}12-trans,\;{\Delta}15-cis,\;and\;C_{18:3}\;{\Delta}9-cis,\;{\Delta}12-cis,\;{\Delta}15-cis$. The formation of trans-fatty acids by deodorization at $240{\sim}280^{\circ}C$ for 2 hrs was in the range of 1.78 to 5.74%. Conclusively, the deodorizing conditions of $240^{\circ}C$ for 2 hrs or $250^{\circ}C$ for 1 hr were suggested as the best conditions which could minimize the formation of trans isomers of fatty acids in soybean oils.

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Hydrogel Synthesis using Glycosyl Methacrylate and Acrylate: 1. A Study on Chemo-Enzymatic Synthesis of Sorbitan Acrylate (배당화 메타크릴레이트와 아크릴에리트를 이용한 하이드로겔의 합성: I. 솔비탄 아크릴레이트의 화학.효소적 합성에 관한 연구)

  • 박돈희;임근길;정귀택;변기영;김인흥;이광연;김해성
    • KSBB Journal
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    • v.18 no.3
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    • pp.222-228
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    • 2003
  • This study was performed to research a chemo-enzymatic synthesis of sorbitan acrylate. It w as firstly to determine the optimum conditions for D-sorbitol cyclic reaction in the presence of p-toluenesulfonic acid (p-TSA) as catalyst material. It was secondly to find the optimum conditions for sorbitan acrylate synthesis using immobilized lipase Novozym 435 in t-butanol from its materials. The maximum yield of 1,4-sorbitan synthesis were obtained approximately 90% (w/w) at 13$0^{\circ}C$ and 200 mmHg vacuum pressure with 1% (w/w) p-TSA after 150 min reactin time on our experimental system. The product from optimum condition was less color than those obtained at higher temperatures and minimized byproduct and unreacted D-sorbitol. Sorbitan acrylate was synthesized to around 63.5% conversion of 1,4-sorbitan. The experimental optimum condition was found at 5$0^{\circ}C$, atmospheric pressure, 3% (w/v) Novozym 435, 50 g/L 1,4-sorbitan of initial reactant concentration, and 1:3 molar ratio of 1,4-sorbitan to acrylic acid.

High Permeability, High Selectivity Carbon-Silica Membranes for Gas Separation (기체분리용 고투과선택성 탄소-실리카막)

  • 이영무;박호범
    • Membrane Journal
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    • v.12 no.2
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    • pp.107-119
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    • 2002
  • Carbon-silica ($C-SiO_2$) membranes can be easily prepared by the pyrolysis of two-phase copolymers containing an aromatic imide block and a siloxane block and remarkably high permselectivities of $He/N_2, O_2/N_2,$ and $CO_2/N_2$. The pyrolysis of the imide-siloxane block copolymers was carried out at different final temperatures, $600^{\circ}C, 800^{\circ}C,$ and $1000^{\circ}C$ under an inert atmosphere, and is the first reported case of the precursors being used for the preparation of carbon membrane. The polymeric precursors were synthesized in a wide range of siloxane content and different final morphology, and the pyrolozed membranes were tested with a high vacuum time-lag method at $25^{\circ}C$ and 76cmHg of feed pressure. In experiments with He, $CO_2, O_2 \;and \;N_2$, the membranes were found to have good $O_2/N_2$ selectivity up to 32.2 and $O_2$ permeability on the order of $10-8/cm^2(STP)cm/cm^2seccmHg.$.

Forged Product Characteristic and Cold Rolling Simulation for High-Nitrogen Stainless Steel (HNS) (TP304계 고질소 스테인레스강의 단조특성과 냉간압연 모사)

  • Lee, M.R.;Lee, J.W.;Kim, B.K.;Kim, Y.D.;Shin, J.H.
    • Proceedings of the Korean Society for Technology of Plasticity Conference
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    • 2009.05a
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    • pp.310-313
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    • 2009
  • Several high nitrogen stainless steel ingots(100kg) were fabricated with changing Ni and $[N]_2$ contents by Pressurized Vacuum Induction Melting(P_VIM). After free forging process, chemical compositions, microstructure and mechanical properties were estimated. Hardness was increased with the increase of $[N]_2$ content. Furthermore, microstructure including a lot of tempering twins was observed with optical microscope. Mechanical properties were estimated as function of solution treatment temperature and cooling method(air/water) under duration time of 1 hr on sample that were fabricated with Ni content under the atmospheric $[N]_2$ pressure. At solution treatment range of $1050{\sim}1100^{\circ}C$, hardness was decreased with the increase of solution temperature and there were little discrepancy of microstructure and hardness with cooling method. Computer simulation was carried out in order to inspect pass schedule in cold rolling process. When the condition of simulation was roll speed of 2.5mpm, rolling rate $15{\sim}17%$ per pass, it was ascertained that the formation such as deformation by sticking and lamellar sliver etc. was restricted from a simulation.

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Fundamental Study on a Distillation Separation of a LiCl-KCl Eutectic Salt from Rare Earth Precipitates (희토류 침전물로부터 LiCl-KCl 공융염의 증류 분리에 관한 기초연구)

  • Yang, Hee-Chul;Eun, Hee-Chul;Kim, In-Tae
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.8 no.1
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    • pp.65-70
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    • 2010
  • The distillation rate on LiCl-KCl eutectic salt under different vacuums from 0.5-50 mmHg was first investigated by using both a non-isothermal and a isothermal thermogravimetric (TG) analysis. Based on the non-isothermal TG data, distillation rate equations as a function of the temperature could be derived. Calculated flux by these model flux equations was in agreement with the distillation rate obtained from isothermal TG analysis. A distillation rate of $10^{-4}-10^{-5}$ mole $cm^{-2}sec^{-1}$ is obtainable at temperatures less than 1300K and vacuums of 0.5-50 mmHg. About a 99% salt distillation efficiency was obtained after an hour at a temperature above 1150 K under 50 mmHg in a small scale distillation test system. An increase in the vaporizing surface area is relatively effective for removing residual salt in the remaining particles, when compared to that for the vaporizing time. Over 99.95% of total distillation efficiency was obtained for a 1-h distillation operation by increasing the inner surface area from $4.52cm^2$ to $12.56cm^2$.

Packaging Techniques to Prevent Winter Kimchi from Inflation (겨울 김치에 대한 팽창 방지 포장 기법)

  • Hong, Seok-In;Park, Noh-Hyun;Park, Wan-Soo
    • Korean Journal of Food Science and Technology
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    • v.28 no.2
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    • pp.285-291
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    • 1996
  • The effect of various packaging methods on Kimchi quality was investigated in order to develop the packaging techniques for preventing commercial Kimchi Products from ination and explosion due to fermentative gas evolved during storage and distribution. Kimchi was packaged in different methods; atmospheric (AP), check-valved (CV), double (DP) and vacuum (VP) packaging. The quality of Kimchi during storage at $10^{\circ}C$ was evaluated ill terms of gas composition, free volume, pH, titratable acidity, color index, lactic acid bacteria and sensory properties. $O_2$ concentration decreased to about 1% at $6{\sim}8$ days of optimal ripening time in all packages except DP, in which it remained around 20%. $CO_2$ concentration reached $70{\sim}90%$ after $6{\sim}8$ days in AP, CV and DP, while it stayed around 10% in DP. The free volume in AP had typical sigmoidal curve similar to $CO_2$ concentration changes. It remained almost constant in CV and DP, but started to increase at the late stage of storage In VP. There was no significant influence of packaging methods on the other quality attributes such as pH, titratable acidity, color index (L.b/a), lactic acid bacteria count and sensory evaluation score. As results, it could be proposed to employ CV and DP method as the effective packaging techniques for preventing commercial Kimchi products from inflation.

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