On-column sampling device for thermogravimetry/capillary gas chromatography/mass spectrometry
A simplified thermogravimetry/gas chromatography/mass spectrometry (TG/GC/MS) system has been developed which completely eliminates the off-line trapping and devolatilization step and the associated sample transfer problems. There are no valves or transfer lines between the TGA furnace and the GC. The gaseous products generated in the TGA are taken from the immediate vicinity of the sample in the furnace and are cryogenically condensed on the front end of a wall-coated open tubular fused silica capillary chromatographic column. This minimizes undesired gas-phase pyrolysis and/or wall reactions in the furnace environment and results in a condensed off-gas sample which is already prepared for chromatographic separation. In addition to the above advantages in sampling the gaseous materials from the TGA furnace, the fused silica capillary column also provides other benefits. It is well known that glass capillary columns give better separations, shorter analysis times, and better sensitivity and are more inert than conventional packed GC columns. The use of these columns also enables one to change from the TG/MS to the TG/GC/MS configuration in a matter of minutes so that both kinds of data may be acquired to better elucidate the nature of thermally induced reactions. 6 references, 9 figures, 2 tables.
- Research Organization:
- Dow Chemical Co., Midland, MI
- OSTI ID:
- 5959553
- Journal Information:
- Anal. Chem.; (United States), Vol. 56:9
- Country of Publication:
- United States
- Language:
- English
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ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
01 COAL, LIGNITE, AND PEAT
COAL
PYROLYSIS
QUANTITATIVE CHEMICAL ANALYSIS
COAL GAS
MASS SPECTROSCOPY
SAMPLING
THERMAL GRAVIMETRIC ANALYSIS
EXPERIMENTAL DATA
GAS ANALYSIS
GAS CHROMATOGRAPHY
SENSITIVITY
CARBONACEOUS MATERIALS
CHEMICAL ANALYSIS
CHEMICAL REACTIONS
CHROMATOGRAPHY
DATA
DECOMPOSITION
ENERGY SOURCES
FLUIDS
FOSSIL FUELS
FUELS
GASES
GRAVIMETRIC ANALYSIS
INFORMATION
MATERIALS
NUMERICAL DATA
SEPARATION PROCESSES
SPECTROSCOPY
THERMAL ANALYSIS
THERMOCHEMICAL PROCESSES
400104* - Spectral Procedures- (-1987)
400102 - Chemical & Spectral Procedures
010600 - Coal
Lignite
& Peat- Properties & Composition