Method Validation for Measurement of Selected Semivolatile Phenols in Dust and Soil

The objectives of this study were to evaluate and validate analytical methods for analysis of persistent organic pollutants (POP) in house dust and soil and to obtain concentration profiles for the target POP in house dust and soil samples from the homes of 13 lowincome families. The analytical method for determining p-pentylphenol, poctylphenol, nonylphenols, and bisphenol-A consisted of sequential extraction of the dust/soil with 5% acetic acid in methanol (MeOH), 100% dichloromethane (DCM), and 5% acetic acid in water; liquid-liquid partitioning the resulting extract with water; and analyzing the concentrated DCM extract by gas chromatography/mass spectrometry (GC/ MS). With this method, quantitative recoveries (>80%) of the target phenols were obtained from the spiked soil samples. Estimated detection limits for the target phenols are 0.001 ppm. The analytical method for 2acetylaminofluorene (2AF) and 3-amino9-ethylcarbazole (AEC) consisted of extracting dust/soil with 30% water in MeOH at pH 10, and analyzing the extract by liquid chromatography with tandem mass spectrometry (LC/MS/MS). Recoveries for 2AF and AEC from the spiked soil samples ranged from 98% to 110% and from 39% to 110%, respectively. Estimated detection limits are 0.001 ppm for 2AF and 0.005 ppm for AEC. The sums of concentrations of target phenols ranged from 1.94 to 14.8 ppm in house dust samples, from 0.047 to 1.51 ppm in entryway dust samples, and from 0.021 to 0.265 ppm in pathway soil samples. The observed concentration trend was house dust > entryway dust > pathway soil. There were no detectable amounts of 2AF and AEC in any dust or soil samples. Other compound classes found in dust and soil samples from one household were alkanes, aliphatic alcohols, fatty acids, fatty acid esters, and phthalates. This Project Summary was developed by EPA’s National Exposure Research Laboratory, Research Triangle Park, NC, to announce key findings of the research project that is fully documented in a separate report of the same title (see Project Report ordering information at back).