An attempt was made to establish a reliable method using chemical neutron activation analysis for surveillance of pollutants in waste waters released by plants manufacturing various kinds of products. Since preconcentration process played important role in the entire course of the analysis work, special precaution was taken to re-confirm that the recovery efficiencies for pollutant ions were satisfactory during the preconcentration. It was also re-examined that the Langmuir's adsorption isotherm pattern well obeyed by all ions under investigation. In recent years, significant amounts of rare earth compounds and other raw materials containing representative elements have been imported and consumed to meet the demand due to the rapid progress in new manufacturing technology. Samples were collected from ten various production lines in plants and potential pollutants were determined using the Tsing Hua Open-pool Reactor. It would be noteworthy that the specimens obtained by this preconcentration process also would be usable for Induced Coupled Plasma-Mass Spectrometry analysis for supplementary and/or comparison purposes.