The aromatic organoarsenic compounds 4-hydroxy 3-nitrobenzenearsenic acid (Roxarsone, ROX) or 4-aminoben-zenearsenic acid (p-arsanilic acid, p-ASA) are used as feed additives in the poultry industry for disease control and enhanced feed efficiency. While federal regulations govern acceptable As concentrations in edible tissue, elevated As concentrations occur in poultry litter, which raises concerns over repeated land application of poultry litter in agriculture. As a precursor to studying the fate of these organoarsenic compounds in soils, three speciation methodologies were developed to separate ROX and p-ASA from the more common and more toxic As species arsenate, arsenite, dimethyl arsenic acid (DMA), and monomethyl arsenic acid (MMA). The six arsenic species were separated on a Dionex AS14 column using a PO4 eluant, an AS16 column using a OH- eluant, and an AS7 column using a HNO3 eluant. While all three methods provided detection limits below 0.5 microg L(-1) for all species, detection limits were lowest for the AS16 and AS7 columns, where all detection limits were generally < 0.05 microg L(-1). The major arsenic species in a water extract of a poultry litter sample was identified as ROX by all three methods with trace concentrations of DMA and As(V) also detected. The AS14 and AS16 separations also revealed a number of unidentified As species present at low concentrations, presumably metabolites of ROX. This methodology should prove useful in identifying organoarsenic compounds and the more toxic inorganic species in soils subject to poultry litter application.