Comprehensive Two-Dimensional GC Analysis of Geological Samples Using Pyrolysis Inlet and Time-of-Flight MS Detection

Physics

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1060 Planetary Geochemistry (5405, 5410, 5704, 5709, 6005, 6008), 6225 Mars, 6297 Instruments And Techniques, 9820 Techniques Applicable In Three Or More Fields

Scientific paper

A pyrolysis inlet-comprehensive two-dimensional GC time-of-flight MS (Pyr-2DGC-TOFMS) system was used to study several groups of rock, soil, and tholin samples. Rock samples studied include limestone, gypsum, and basalt with varying particle sizes. Many different soil samples were studied from varying locations and under varying conditions. The tholins studied are a synthetic analogue to the solid organic materials that are responsible for the thick haze that surrounds Titan, the largest moon of Saturn, and are thought to have been present in the early Earth atmosphere. These mixtures represent a unique and complex application for 2DGC due to the high number of components with a wide range of volatility and polarity. In this study we use Pyr-2DGC-TOFMS to separate and characterize sample components. Using this chromatographic method, two capillary columns are connected in series with a thermal modulator at the junction point. The first column, a relatively long column with a non-polar stationary phase, is used to separate components based primarily on their boiling point. The second column, a short column with a polar stationary phase, allows for a quick separation based on polarity. A two-stage thermal modulator at the column junction point uses a liquid nitrogen-cooled jet to trap and focus components as they come off the first column and then injects them into the second column as a narrow plug using a hot air jet. The two-dimensional separation increases the chromatographic peak capacity and allows for increased sensitivity for trace components. The highly structured chromatograms provided by 2DGC allow for the prediction of peak locations in the retention plane and aid in peak identification. When coupled with a TOF-MS detector the 2DGC is a powerful tool for the separation and identification of the 1000+ peaks that are seen in these rock, soil, and tholin samples. Pyrolysis is the ideal sample introduction system for these samples since they contain high molecular weight compounds and are not soluble in most organic solvents. Information collected by these experiments will contribute to the analysis of pyrolysis and GC/MS data collected by the current Cassini-Huygens mission to Saturn and Titan that will reach its destination in the summer of 2004. In addition, this work will contribute to the instrumental and experimental designs for proposed instrument packages for future missions to the surface of Mars.

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