| Project/Area Number |
13640610
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| Research Category |
Grant-in-Aid for Scientific Research (C)
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| Allocation Type | Single-year Grants |
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| Section | 一般 |
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| Research Field |
分離・精製・検出法
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| Research Institution | Kansai University |
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Principal Investigator |
ARAKAWA Ryuichi Kansai University, Department of Engineering, Prof., 工学部, 教授 (00127177)
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| Project Period (FY) |
2001 – 2003
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| Project Status |
Completed (Fiscal Year 2003)
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| Budget Amount *help |
¥2,900,000 (Direct Cost: ¥2,900,000)
Fiscal Year 2003: ¥600,000 (Direct Cost: ¥600,000)
Fiscal Year 2002: ¥600,000 (Direct Cost: ¥600,000)
Fiscal Year 2001: ¥1,700,000 (Direct Cost: ¥1,700,000)
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| Keywords | electrospray ionization / ESI-MS / on-line analysis / supercritical fluid / SCF / intermediates / propylene oxide / propylene carbonate / prolene carbonate |
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| Research Abstract |
Electrospray ionization mass spectrometry (ESI-MS) is a soft ionization process that provides a simple mass spectrum with little fragmentation. We have developed on-line ESI-MS by interfacing immediately upstream of the electrospray needle with several types of micro-cell. The cells used include photochemical reaction cells, electrolysis cells and low-temperature reaction cells. These cells were used to study the on-line photochemical reaction or electrolysis reaction of metal complexes in solution. By on-line ESI-MS analysis we have detected the reaction intermediates formed in the reaction cells, and clarified the reaction mechanism. In a present study we seek to develop an interface of a supercritical fluid (SCF) reaction with ESI-MS for on-line analysis, and to characterize the unstable chemical species that are formed in the SCF reaction. To achieving rapid and high-sensitivity on-line detection of the SCF reaction products it is vital to develop an ESI interface that matches the optimum conditions of the ESI process.
The on-line method was developed for direct analysis of synthesis reactions in CO_2 SCF by the installation of a compact SCF reaction cell and the ESI interface with MS. The introduction reactions of carbon dioxide described below were studied using catalysts of various alkali halides in supercritical carbon dioxide (scCO_2). The performance of the ESI interface was examined.
1.propylene oxide(PO)→propylene carbonate(PC)
2.1,2-Butylene Oxide(BO)→1,2-Butylene Carbonate(BC)
The primary reaction products and catalytic effect of alkali halides were examined by scCO2-ESI-MS. The results indicated that sodium iodide had the greatest catalytic effect among them. A tendency of the effect was discussed from difference of ion radius between alkaline metal and halogen, or difference in electronegativity of halogens. ESI-MS was a useful technique to analyze carbonate compounds formed by scCO2 reaction.
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