The objectives of this study were to evaluate and validate analytical methods for analysis of persistent organic pollutants (POP) in dust/soil and to obtain concentration profiles for the target POP in dust/soil samples from the homes of 13 low-income families. The analytical method for determining p-pentylphenol, p-octylphenol, nonylphenols, and bisphenol-A consisted of sequential extractions of the dust/soil with 5 percent acid in methanol (MeOH), 100 percent dichloromethane (DCM), and 5 percent 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). The analytical method for determining 2-acetylaminofluorene (2AF) and 3-amino-9-ethylcarbazole (AEC) consisted of extracting dust/oil with 30 percent water in MeOH at pH 10, and analyzing the extract by liquid chromatography with tandem mass spectrometry (LC/MS/MS). The observed concentrations trend was house dust > entryway dust > pathway soil. Other compound classes found in dust/soil samples from one household were alkanes, aliphatic alcohols, fatty acids, fatty acid esters, and phthalates.