Development and Evaluation of Supercritical Fluid Chromatography/Mass Spectrometry for Polar and High-Molecular-Weight Coal Components. Technical Progress Report

摘要

This Technical Progress Report reviews the technical progress made over the first 18 months of the program. Our goals include the design, development, and evaluation of a combined capillary column supercritical fluid chromatograph/high-performance mass spectrometer capable of analyzing high-molecular-weight polar materials and evaluating the system's potential for application in coal conversion process monitoring. The program includes not only the development and evaluation of the required instrumentation, but the development of polar fluids and compatible chromatographic stationary phases needed for efficient separation and analysis of polar and high-molecular-weight compounds. A new chromatograph/mass spectrometer interface and new mass spectrometer ion source have been designed, constructed, and evaluated using low-polarity supercritical fluids such as pentane. Results from the evaluations have been used to modify the instrumentation to improve performance. The design and fabrication of capillary flow restrictors from fused silica tubing has been explored. Research has also been conducted toward advancing the technology of fabricating high-performance chromatographic columns suitable for use with polar supercritical fluids. Results to date support our initial belief that high-resolution supercritical fluid chromatography (SFC)/high-performance mass spectrometry (MS) will provide a significantly enhanced analytical capability for broad classes of previously intractable fuel components. 10 refs., 13 figs. (ERA citation 11:019026)