A Study of Chromatographic Resolution of Enantiomers: Solvent Characteristics of Supercritical Fluid and Liquefied Gas
| Project/Area Number |
62550696
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| Research Category |
Grant-in-Aid for General Scientific Research (C)
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| Allocation Type | Single-year Grants |
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| Research Field |
化学工学
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| Research Institution | Osaka University |
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Principal Investigator |
NITTA Tomoshige Osaka University, Faculty of Engineering Science, Associate Professor, 基礎工学部, 助教授 (00029480)
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| Project Period (FY) |
1987 – 1988
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| Project Status |
Completed (Fiscal Year 1988)
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| Budget Amount *help |
¥1,900,000 (Direct Cost: ¥1,900,000)
Fiscal Year 1988: ¥300,000 (Direct Cost: ¥300,000)
Fiscal Year 1987: ¥1,600,000 (Direct Cost: ¥1,600,000)
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| Keywords | Supercritical Fluid / Chromatography / Optical Resolution / Liquefied Gas / Carbon Dioxide / Propane / Cellulose Derivative / 粒内拡散抵抗 / 溶媒効果 / 分離係数 / 理論段相当高さ / セルロース誘導体 / 分離能 / 保持容量 |
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| Research Abstract |
The present work concerns with the separation characteristics of the supercritical carbon dioxide and liquified propane as a mobile phase in chromatographic resolution of potically active isomers. Two enantiomers, trans-stilbene oxide and 1-(9-anthryl)-2,2,2-trifluoroethanol, were resolved by a column with a chiralcellulose derivative coated on a silica gel. The experimental results are summarized as follows.
(1) Carbon dioxide, propane and hexane are in the order of high resolution; the order is in parallel to the diffusivity in each solvent.
(2) The capacity ratio decreases with increasing the concentration of alcohols for the three solvents. It also decreases with increasing pressure in case of the supercritical fluid. These observations may be explained by the competitive adsorptions of solute and solvent molecules on active sites.
(3) The separation factor significantly increases with decreasing temperature, and it changes a little according to the combination of major fluids and add
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ed alcohols. The relative stability of adsorbed enantiomers may be controlled majorly by the solutes-polymer interactions and secondly by the solutes-solvents interactions in the adsorbed phase.
(4) The separation factor of enantiomers increases slightly with increasing pressure of the supercritical fluid, which corresponds to the decrease of alcohol concentration in the adsorbed phase.
(5) In a low velocity region where molecular diffusion and fluid-mixing are predominant, the overall mass transfer resistance for polymer-coated silica gel is smaller than that for the naked gel; however, in a high velocity region, the polymer-coated silica gel shows higher resistance than the naked. There may be two plausible explanations: 1) increase of the tortuosity factor in the porous particle due to the inclusion of polymers 2) particle coalescence due to the polymers attached on the outside of particles. The fundamental research on polymer coating method will be necessary for improving column efficiency. Less
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Report
(3 results)
Research Products
(6 results)
