The chemical form or speciation of Hg in the floodplain soils of the East Fork Poplar Creek in Oak Ridge TN, a site contaminated from past industrial activity, was investigated. Hg speciation in the soils is an important factor in controlling the fate and effect of mercury at the site and in assessing human health and ecological risk. Application of 3 different sequential extraction speciation schemes indicated the Hg at the site was predominantly relatively insoluble mercuric sulfide or metallic Hg, though the relative proportions of each did not agree well between procedures. Application of x-ray and electron beam studies to site soils confirmed the presence of metacinnabar, a form of mercuric sulfide, the first known evidence of authigenic mercuric sulfide formation in soils