In the early 1950's, a federal facility in Oak Ridge, Tennessee, used a process that required the use of Hg to produce8Li. It was disclosed to the public in 1983 that about 2.4 millions pounds of Hg had been released into the ecosystem. The primary route of mercury into the environment was a stream, East Fork Poplar Creek, whose head waters are in the vicinity of the plant. As part of a study to determine the distribution of Hg as well as As, Cr, Sb, Se, U, and Zn along the flood plains of the creek, a procedure using neutron activation analysis was developed and is described below. The procedure, typical sample analysis results for Hg, and quality assurance and control data are discussed in this paper.