This study was undertaken to develop an improved method for determining the total content of individual semivolatile organic compounds in solid wastes. The requirements of the method are as follows: applicable to a wide range of specimen matrixes; applicable to a wide range of compounds; quantification range of 1 ppm to 100%; acceptable recovery and reproducibility; and easily performed at reasonable cost.
The waste matrixes of interest include aqueous sludges, dry solids, soils, tars, oils, and oily sludges. The compounds of interest include aromatic halocarbons, aromatic hydrocarbons, aromatic nitro compounds, chlorinated pesticides, phosphates esters, halogenated ethers, phenols, anilines, quinolines, and other extractable organic compounds having boiling points in the range of 150 to 500°C.
The method developed is a dry neutral extraction procedure that involves a single extraction with methylene chloride under neutral conditions with anhydrous sodium sulfate added to remove any water present. Sonification with a high-intensity sonic probe is used to promote the interaction of the extraction solvent with the waste. Screening steps are incorporated into the method to determine the neutralization requirement of the specimen, the residue weight of the extract, and the optimum concentration of the extract for subsequent analysis. Gas chromatography-mass spectrometry (GC-MS) analysis using a fused silica capillary column is used to analyze the extract.
The dry neutral extraction method shows promise in meeting the requirements specified. The estimated quantification limit is 1 ppm for specimens that contain up to 1 mg/g of solvent extractable material and proportionately higher for other specimens. The mild extraction conditions used mimimize any losses from chemical reactivity. No emulsion or phase separation problems are encountered. The use of a single extraction under neutral conditions as employed in the method has been shown to be suitable for the extraction of a wide variety of compounds including phenols, anilines, and neutral compounds.
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