A preconcentration method combined with neutron activation technique for the analysis of organic and inorganic mercury in waste water samples at ppb levels is presented. The inorganic mercury is extracted in CCl4 solution with lead diethyldithiocarbamate reagent and the organic mercury is extracted in C6H6 solution. Interfering activities of sodium and bromine are removed from the irradiated samples by this procedure. Two different solvent extraction procedures are also described in detail.