Development and Applications of an Automated In-Column Pyrolysis Gas Chromatography-Mass Spectrometry System |
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Authors: | D Beyer P Eckerle H Cortes W Engewald K Dettmer |
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Institution: | 1. Dow Olefinverbund GmbH, R&D Analytical Sciences, Building F 17, 06258, Schkopau, Germany 2. Dow Deutschland GmbH&OHG, R&D Analytical Sciences, Building B.3.4, 77834, Rheinmünster/Greffern, Germany 3. The Dow Chemical Company, Analytical Core Technologies, Building 1897, 48667, Midland, MI, USA 4. Institute of Analytical Chemistry, University of Leipzig, Linnéstra?e 3, 04103, Leipzig, Germany 5. University of California at Davis, 1-Shields Avenue, Davis, CA, 95616, USA
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Abstract: | A novel system for sample introduction into a Gas Chromatograph (GC) using an automated in-column pyrolysis device has been
developed. The in-column pyrolysis device is suitable for use with any GC or GC-MS system. Solid samples are dissolved or
emulsions can be diluted and injected into the system. Because the system is designed for introducing liquid samples, a better
control of the injected sample amounts is achieved. This leads to high reproducibility of the peak areas, offering new opportunities
for quantitation of polymers or other high molecular weight materials. In addition, a better statistical representation of
the material to be analyzed is given if the samples are dissolved in a solvent. The system can be operated both in a normal
GC injection mode, and in the pyrolysis mode. As a conventional GC injector working in on-column or Programmed Temperature
Vaporization (PTV) injection mode, (without the pyrolysis function), information on the volatile fraction of a sample can
be obtained. Once the volatile materials in the sample have been separated, a second analysis on the non-volatile matrix can
be performed by initiating the pyrolysis sequence, yielding information on the non-volatile fraction of the sample. Both features,
on column or PTV injection mode and in-column pyrolysis can be used separately or in combination. This new technology is expected
to be useful for the determination of additives, monomers, solvents and other volatile components in a non volatile matrix,
such as polymers, as well as in the characterization of the non-volatile matrix itself, in a single run.
Revised: 20 June and 21 July 2005 |
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Keywords: | Gas chromatography-mass spectrometry Automated in-column pyrolysis Additives and solvents Polymer matrices |
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