• 제목/요약/키워드: Solid Separation

검색결과 504건 처리시간 0.029초

Chiral Mesoporous Silica for Asymmetric Metal-free Catalysis: Enhancement of Chirality thorough Confinement Space by Plug Effect

  • 정은영;임청래;박상언
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2011년도 제41회 하계 정기 학술대회 초록집
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    • pp.199-199
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    • 2011
  • The addition of a carbanion to ${\yen}{\acute{a}}{\yen}{\hat{a}}$-unsaturated carbonyl compounds is of importance in the C-C bond formation reactions for modern pharmaceuticals and organic synthesis. Recently, heterogeneous asymmetric catalysis became more attractive area of research because of the easy recovery and separation of the catalyst from the reaction system. Most of synthetic methods for heterogeneous catalysts were grafting or immobilization of homogeneous catalyst onto the solid supports. Trans-1,2-Diaminocyclohexane(DACH) and L-proline ligands have been enormously used as chiral ligands in several catalytic transformation under homogenous conditions. Our group prepared l-proline functionalized mesoporous silica was synthesized under acidic condition using a poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer template (EO20PO70EO20, Pluronic P-123, BASF). Furthermore, we successfully directly synthesized trans-1,2 diaminocyclohexane functionalized mesoporous silica by using microwave method. The direct functionalization of chiral ligand into the framework of mesoporous materials is expected to be useful for the heterogeneous asymmetric catalysis. So, we adopt the direct synthesis of chiral ligand functionalized mesoporous silica by using thermal and microwave irradiation. Then, chiral ligand functionalized mesoporous silicas were applied to enantioselective asymmetric catalytic reactions.

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GC-MS/MS와 LC-MS/MS를 이용한 생약재 중 261종 농약의 동시분석 (Development of Multi-residue Analytical Method for 261 Pesticides in Herbal Medicines using GC-MS/MS and LC-MS/MS)

  • 나은식;김성수;홍성수;김경주;이용재;이병철;이규승
    • 한국환경농학회지
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    • 제39권2호
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    • pp.142-169
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    • 2020
  • BACKGROUND: A new analytical method has been developed to determine 261 pesticide residues in herbal medicines. METHODS AND RESULTS: The extraction of pesticides was carried out by modified method of the Korea Food Standards Codex sample extraction and determination was performed using GC-MS/MS and LC-MS/MS. During the pre-treatment process of the test method, Solid-liquid separation was changed to centrifugation. The method was validated by the precision and accuracy results. 261 pesticides spiked at three level 20, 50, 100 ug/kg in herbal medicines. The limit of quantification of method were 4-40 ug/kg for GC-MS/MS and 2-45 ug/kg for LC-MS/MS, respectively. Among the pesticides analysed by GC-MS/MS and LC-MS/MS, 244 pesticides (94% of total number) in chinese matrimony vine and 224 pesticides (86% of total number) in korean angelica root and 231 pesticides (89% of total number) in jujube and 214 (82% of total number) in cnidium showed recoveries in the range of 70-120% with RSD⪯20%. CONCLUSION: These results indicated that GC-MS/MS and LC-MS/MS analysis with the sample extraction in this study can be applied to multi-residue analysis of pesticides in herbal medicines.

연속냉각 중 과냉 된 $Pd_{40}Cu_{30}Ni_{10}P_{20}$ 합금 용탕의 실시간 응고거동 관찰 (In Situ Observation of Solidification Behavior in Undercooled $Pd_{40}Cu_{30}Ni_{10}P_{20}$ Alloy Melts during Linear Cooling)

  • 김지훈
    • 한국주조공학회지
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    • 제23권5호
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    • pp.276-285
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    • 2003
  • In the undercooled melt of $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy, the solidification behavior including nucleation and growth of crystals at the micrometer level has been observed in-situ by use of a confocal scanning laser microscope combined with an infrared image furnace. The $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy specimens were cooled from the liquid state to glass transition temperature. 575 K, at various cooling late under a helium gas flow. According to the cooling rate, the morphologies of the solidification front are changed among various types, irregular jog like front, columnar dendritic front, cellular grain, star like shape jog and fine grain, etc. The velocities of the solid-liquid interface are measured to be $10^{-5}{\sim}10^{-8}$ m/s which are at least two orders higher than the theoretical crystal growth rates. Combining the morphologies observed in terms of cooling rates and their solidification behaviors, we conclude that phase separation takes place in the undercooled molten $Pd_{40}Cu_{30}Ni_{10}P_{20}$ alloy. The continuous cooling transformation (CCT) diagram was constructed from solidification onset time at various linear cooling conditions with different rate. The CCT diagram suggests that the critical cooling rate for glassy solidification is about 1.5 K/s, which is in agreement with the previous calorimetric findings.

이중유벽의 유효성에 관한 해석 (Analysis of Effectiveness of Tandem Oil Fences)

  • 한동기;이정묵
    • 한국해양환경ㆍ에너지학회지
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    • 제4권1호
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    • pp.38-46
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    • 2001
  • 조류 중에 설치한 이중 유벽의 유효성을 검증하기 위하여 유벽 전후 및 유벽사이에서의 유적(oil droplet)의 거동을 실험적 및 수치적으로 연구하였다. 이 연구에는 단일 유벽의 경우 유벽의 유연성이 포유성능에 미치는 영향도 포함되었다. 실험은 유적의 밀도와 근사한 구형의 고체입자가 전방 유벽의 상류 한 지점에서 방류되었을 때 그 궤적을 추적하는 것이 내용이었다. 입자는 방류되었을 때 유동장의 상태에 따라 자유표면으로 부상하거나, 유벽에 충돌 또는 유벽하로 빠져나가는 현상을 나타내게 된다. 본 논문에는 이러한 유적의 이동 경위를 해석함으로써, 이러한 유적의 유적이 운동을 시작하는 영역이 어딘가에 따라 전방유벽하로 기름이 누출될 것인지 아닌지를 판단할 수 있는 방법과 전후 유벽의 흘수의 차 그리고 수심이 이중유벽의 포유성능에 미치는 영향을 해석할 수 있는 방법을 제시하였다.

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Purple Membrane과 β-carotene에서 산란과 파동전파에 관한 연구 (A Study on Wave Propagation and Scattering in Purple Membrane and β-carotene)

  • 김기준;박태술;성완모
    • 한국응용과학기술학회지
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    • 제33권1호
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    • pp.136-142
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    • 2016
  • 무질서 매질에서 형광, 산란과 응집의 영향은 파장과 산란된 형광세기로 나타내는데, laser induced fluorescence(LIF) 분광학에 의한 분자특성으로 나타난다. 산란매질에서 광학적 효과는 광학적 파라미터들(${\mu}_s$, ${\mu}_a$, ${\mu}_t$)에 의해 표현되고 응집은 고-액상 분리공정과 Photodynamic therapy에서 중요하게 활용되고 있다. 따라서 입자가 서로 접근될 때 콜로이드 입자들의 상호작용을 LIF와 응집효과로 분석하였다. 우리는 레이저 광원에서 검출기까지 거리의 함수에 의해 in vitro 시료의 산란과 형광 스펙트라를 측정하였다. 산란계수 ${\mu}_s$는 산란체의 입자가 증가함에 크게 나타났다. 그리하여 purple membrane vesicle과 ${\beta}$-carotene의 혼합물의 매질에서 광원에서 검출기에 의한 거리에 대한 측정된 값(I, ${\delta}$)이 거리가 가까워짐에 따라 크게 나타났다.

Development of Isotope Dilution-Liquid Chromatography/Tandem Mass Spectrometry as a Candidate Reference Method for the Determination of Acrylamide in Potato Chips

  • Park, Sun-Young;Kim, Byung-Joo;So, Hun-Young;Kim, Yeong-Joon;Kim, Jeong-Kwon
    • Bulletin of the Korean Chemical Society
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    • 제28권5호
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    • pp.737-744
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    • 2007
  • An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of acrylamide in potato chips, starch-rich foodstuff cooked at high temperature. Sample was spiked with 13C3-acrylamide and then extracted with water. The extract was further cleaned up with an Oasis HLB solid-phase extraction (SPE) cartridge and an Oasis mixed-phase cation exchange (MCX) SPE cartridge. The extract was analyzed by using LC/ESI/Tandem MS in positive ion mode. LC with a medium reversed-phase (C4) column was optimized to obtain adequate chromatographic retention and separation of acrylamide. MS was operated to selectively monitor [M+H]+ ions of the analyte and its isotope analogue at m/z 72 and m/z 75, respectively. Sample was also analyzed by the LC/MS with selectively monitoring the collisionally induced dissociation channels of m/z 72 → m/z 55 and m/z 75 → 58. Compared to the LC/MS chromatograms, the LC/MS/MS chromatograms showed substantially reduced background chemical noises coming from solvent clusters formed during ESI spray processes and interferences from sample matrix. Repeatability and reproducibility studies showed that the LC/MS/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0% while the LC/MS results are influenced by chemical interferences.

Modified glycine-nitrate process(MGNP)로 합성한 BaCo1-x-yFexZryO3-δ 산소투과도 및 수소생산성 (Oxygen Permeation and Hydrogen Production of BaCo1-x-yFexZryO3-δ by a Modified Glycine-nitrate Process (MGNP))

  • 이은정;황해진
    • 한국수소및신에너지학회논문집
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    • 제24권1호
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    • pp.29-35
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    • 2013
  • A dense mixed ionic and electronic conducting ceramic membrane is one of the most promising materials because it can be used for separation of oxygen from the mixture gas. The $ABO_3$ perovskite structure shows high chemical stability at high temperatures under reduction and oxidation atmospheres. $BaCo_{1-x-y}Fe_xZr_yO_{3-{\delta}}$ (BCFZ) was well-known material as high mechanical strength, low thermal conductivity and stability in the high valence state. Glycine Nitrate Process (GNP) is rapid and effective method for powder synthesis using glycine as a fuel and show higher product crystallinity compared to solid state reaction and citrate-EDTA method. BCFZ was fabricated by modified glycine nitrate process. In order to control the burn-up reaction, $NH_4NO_3$ was used as extra nitrate. According to X-Ray Diffraction (XRD) results, BCFZ was single phase regardless of Zr dopants from y=0.1 to 0.3 on B sites. The green compacts were sintered at $1200^{\circ}C$ for 2 hours. Oxygen permeability, methane partial oxidation rate and hydrogen production ability of the membranes were characterized by using Micro Gas Chromatography (Micro GC) under various condition. The high oxygen permeation flux of BCFZ 1-451 was about $1ml{\cdot}cm^{-2}s^{-1}$. Using the humidified Argon gas, BCFZ 1-433 produced hydrogen about $1ml{\cdot}cm^{-2}s^{-1}$.

고에너지 밀링을 통한 Ni-BaCe0.9Y0.1O3-δ 서멧 멤브레인의 미세구조 균질성 향상 (Improved Microstructural Homogeneity of Ni-BCY Cermets Membrane via High-Energy Milling)

  • 김혜진;안기용;김보영;이종흔;정용재;김혜령;이종호
    • 한국세라믹학회지
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    • 제49권6호
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    • pp.648-653
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    • 2012
  • Hybridization of dense ceramic membranes for hydrogen separation with an electronically conductive metallic phase is normally utilized to enhance the hydrogen permeation flux and thereby to increase the production efficiency of hydrogen. In this study, we developed a nickel and proton conducting oxide ($BaCe_{0.9}Y_{0.1}O_{3-{\delta}}$: BCY) based cermet (ceramic-metal composites) membrane. Focused on the general criteria in that the hydrogen permeation properties of a cermet membrane depend on its microstructural features, such as the grain size and the homogeneity of the mix, we tried to optimize the microstructure of Ni-BCY cermets by controlling the fabrication condition. The Ni-BCY composite powder was synthesized via a solid-state reaction using $2NiCO_3{\cdot}3Ni(OH)_2{\cdot}4H_2O$, $BaCeO_3$, $CeO_2$ and $Y_2O_3$ as a starting material. To optimize the mixing scale and homogeneity of the composite powder, we employed a high-energy milling process. With this high-energy milled composite powder, we could fabricate a fine-grained dense membrane with an excellent level of mixing homogeneity. This controlled Ni-BCY cermet membrane showed higher hydrogen permeability compared to uncontrolled Ni-BCY cermets created with a conventionally ball-milled composite powder.

Ar-H2플라즈마 건식제련과 마이크로웨이브침출을 통한 지르콘샌드로부터 고순도 지르코니아 분리 (Separation Technology of Pure Zirconia from Zirconsand by the Ar-H2 Arc Plasma Fusion and Sulfuric Acid Leaching with Microwave Irradiation)

  • 이정한;홍성길
    • 자원리싸이클링
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    • 제25권3호
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    • pp.49-54
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    • 2016
  • 본 연구에서는, 아크 플라즈마 정련을 이용하여 지르콘샌드($ZrSiO_4$)를 지르코니아($ZrO_2$)와 실리카($SiO_2$)로 분리하였다. 실리카를 마이크로웨이브 침출을 통해 제거하고 고순도의 지르코니아를 얻었다. 플라즈마 퓨전은 두 가지 공정을 순차적으로 진행하였다. Ar 100% 분위기에서 환원 공정을 거친 후, Ar-$H_2$ 혼합 가스를 통해 정련과정을 거쳤다. 진공 챔버 내에서 냉각 후 지르코니아와 실리카로 이루어진 고상을 얻었다. 마이크로웨이브 침출을 위해 $240^{\circ}C$, 20% 황산용액을 사용하였다. 분석 결과 고순도(98.6%)의 지르코니아를 얻을 수 있었다.

석회석을 이용한 지하수 철분 산화 (Iron Oxidation using Limestone in Groundwater)

  • 심상준;강창덕;이지훤;조영상
    • 대한환경공학회지
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    • 제22권1호
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    • pp.73-81
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    • 2000
  • 지하수 내의 철분 제거를 위해 일반적으로 포기법과 화학적 산화제를 이용한 산화법이 이용된다. 특히 오염수 포기에 이은 고-액 여과 분리 공정은 가장 널리 이용되는 물리 화학적 처리법이다. 이 방법은 주로 pH 6.5 이상의 경우 산화 제1철의 불용화에 매우 효과적인 것으로 알려져 있다. 본 연구에서는 석회석을 일정한 포기 하에 오염수와 접촉시켜 pH를 6.5 이상으로 유지하였다. 회분식 실험에서 석회석 입도 크기, 초기 철분 농도, pH, 온도 및 이온 세기 등에 의한 산화 제1철의 산화속도 변화를 고찰하였다. 석회석의 입도가 감소할수록 pH의 증가가 두드러지며 철분 산화 또한 급격히 증가함을 알 수 있었다. 산화 제1철의 산화속도는 초기 철분 농도, 온도 및 이온세기에 비례하는 것으로 나타났다.

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