On-line analysis of reaction products in CO2 supercritical fluid using electrospray ionization mass spectrometry

使用电喷雾电离质谱在线分析 CO2 超临界流体中的反应产物

基本信息

批准号：
13640610
负责人：
ARAKAWA Ryuichi
金额：
$ 1.86万
依托单位：
Kansai University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2001
资助国家：
日本
起止时间：
2001 至 2003
项目状态：
已结题

项目摘要

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.

电喷雾电离质谱法（ESI-MS）是一个软电离过程，可提供简单的质谱，几乎没有碎片化。我们通过将电喷雾针的上游与几种类型的微电池连接到在线ESI-MS。所使用的细胞包括光化学反应细胞，电解细胞和低温反应细胞。这些细胞用于研究金属复合物在溶液中的在线光化学反应或电解反应。通过在线ESI-MS分析，我们检测到反应细胞中形成的反应中间体，并阐明了反应机理。在本研究中，我们试图开发与ESI-MS的超临界流体（SCF）反应的界面进行在线分析，并表征SCF反应中形成的不稳定的化学物种。为了实现SCF反应产品的快速和高敏性在线检测，开发与ESI过程最佳条件相匹配的ESI界面至关重要。开发了在线方法，通过安装紧凑型SCF反应细胞和与MS的ESI接口直接分析CO_2 SCF中的合成反应。在超临界二氧化碳（SCCO_2）中使用各种碱卤化物的催化剂（SCCO_2）研究了以下描述的二氧化碳的引入反应。检查了ESI界面的性能。1。丙烷氧化物（PO）→碳酸丙酸丙酸丙二醇苯甲酸丙烷（PC）2.1,1,2-22-22-12-2-2-2-2-2-2-2-2-丁烯碳酸盐（BC）。结果表明，碘化钠之间具有最大的催化作用。从合金金属和卤素之间的离子半径差或卤素的电负性差异中讨论了效果的趋势。 ESI-MS是一种有用的技术，用于分析由SCCO2反应形成的碳酸盐化合物。