Author
Reeves Iii, James | |
Francis, Barry | |
McCarty, Gregory |
Submitted to: Pittsburgh Conference
Publication Type: Abstract Only Publication Acceptance Date: 3/11/1999 Publication Date: N/A Citation: N/A Interpretive Summary: Technical Abstract: Pyrolysis-gas chromatography mass spectrometry is widely used to study the composition of a wide range of materials, including forages and soils. Due to the high organic matter content in most samples, relatively small samples are used (i.e., 0.5 mg or less) combined with high split ratios (100 to one or higher) to avoid overloading the mass spectrometer (MS). In addition, the pyrolysis conditions used were often developed when pyrolysis units of limited programmability were the norm. In the course of studying low organic matter soils (total C contents of 0.6 to 3.4%), a new investigation was undertaken for optimizing pyrolysis conditions. Results showed that splitless GC operation was required to obtain sufficient signal from the MS, and that under splitless conditions residues on pyrolysis tubes from fingerprints and dust were detectable, requiring extreme care, including special cleaning of pyrolysis tubes and quartz wool, to produce accurate results, free from external contaminates. Results using a variety of pyrolysis conditions indicate that the maximum amount of information is obtained by using a programmed pyrolysis run. For example, for soils, it was found that information from carbohydrates and lignin is best obtained at pyrolysis temperatures close to 600o C as standardly used for forages, while information from humic substances is better obtained at temperatures near 1000o C. To obtain information on both fractions a programed run from 200 to 1000o C was found to be most advantageous. Similar investigations have now also been undertaken utilizing forages. |