Arsenic and selenium distributions in coal-fired plant samples are studied. This research includes arsenic and selenium concentrations in samples of coal, fly ash, bottom ash, economizer ash, Flue Gas Desulfurization (FGD) slurry and flue gas taken from four power plants with the goal being to examine the distribution of these metals in these materials and calculate a materials balance for the system. All samples were analyzed using ICP-ES. This research shows that 60-80% of the arsenic in coal-fired plant samples will be associated with the fly ash. Approximately 35-55% of the selenium will be associated with the fly ash and approximately 30-40% will be associated with the FGD slurry materials. The amount of arsenic and selenium present in the flue gases escaping the stack is very little, 6-7% or less. Hopefully, research in this area will be helpful when setting emissions limits, identifying and disposing of hazardous wastes and improving air pollution control devices for maximum metal removal.