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Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
38, Number 3, March 2000, pp. 117121
Analysis
of Tetrahydrofuran and Methanol in Distillation Residue Samples by Automated
Headspace Solid-Phase MicroextractionGas Chromatography with Flame Ionization
Detection
Walter
K. Gavlick
Monsanto, 800 North Lindbergh Blvd., St. Louis,
MO 63167
Automated headspace
solid-phase microextraction (SPME) coupled with gas chromatography and flame
ionization detection is used to determine the amounts of methanol and tetrahydrofuran
(THF) in distillation residue samples from a proprietary chemical reaction.
A 65-µm polydimethylsiloxane/divinylbenzene SPME fiber is used to perform
the extractions. Optimized extraction conditions for each analyte are determined
using a parts-per-million-level methanol in water standard and a parts-per-billion-level
THF in water standard. The amount of methanol and THF in distillation residue
samples is quantitated by both standard addition and external standard calibration
curve. The two methods of quantitation are compared.
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