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Interim Protocol for the Automated Analysis of Semivolatile Organic Compounds by Gas Chromatography/Fourier Transform Infrared (GC/FT-IR) Spectrometry

Volume 39, Number 5 (Oct. 1985) Page 827-833

Gurka, Donald F.

The application of gas chromatography/Fourier transform infrared (GC/FT-IR) data to regulatory decisions requires, among other things, the availability of validated analytical protocols. Such protocols are necessary for the generation of reliable analytical data. A GC/FT-IR protocol is described which is applicable to the determination of semivolatile organic compounds in wastewater, soils, sediments, and solid wastes. The protocol is designed for the high-throughput automated analysis of multicomponent environmental and hazardous waste extracts. Wastewater analysis for semivolatile organic compounds is based upon the extraction of 1 L of sample with methylene chloride and the concentration of the extract to 1 mL. The analysis of the semivolatile fraction derived from solid waste analysis is based upon the extraction of 50 grams of sample and concentration of the sample extract to 1.0 mL. A gel permeation cleanup option is included to further purify those extracts which cannot be concentrated to the specified final volume. With the use of capillary GC/FT-IR techniques, wastewater identification limits of 150 to 400 ppb can be achieved with this method, while the corresponding identification limits for solid samples are 3 to 88 ppm. Automated packed-column GC/FT-IR identification limits are approximately a factor of five higher than the corresponding capillary GC/FT-IR values. The most frequent obstacle to the achievement of these identification limits is expected to be the presence of large quantities of interfering high-boiling coextractants. These coextractants would raise the identification limits by preventing the concentration of extracts to the desired final volume, thereby necessitating gel permeation cleanup, and/or by decreasing the spectral signal-to-noise of GC-volatile analytes by raising the spectral background intensity.