During the present work rare earth elements (REEs) in Periyar River water and in seawater from the region of Mumbai, India, have been measured via neutron activation analysis. To separate and concentrate REEs a pre-irradiation separation approach via ion exchange was adopted. Standard addition and radiotracer studies were carried out to validate the analytical methodology including the recoveries of the separations. The measured REE concentrations in the water samples are presented and discussed.