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The present study was oriented to prepare new scintillating anion-exchange resins for measurement of 99TcO4- in natural waters. The organic fluor 2-(1-naphthyl)-5-phenyloxazole was diffused into (chloromethyl)polystyrene resin. Thereafter, a thin layer of poly[[2-(methacryloyloxy)ethyl]trimethylammonium chloride] was grafted from the resin surface by surface-initiated atom transfer radical polymerization as an attempt to overcome potential problems related to the leaching of fluor molecules during usage. The residual chloromethyl groups of the polymer-coated resin were aminated by reaction with two different tertiary amines, triethylamine (TEA) and methyldioctylamine (MDOA). Off- and on-line quantification of 99Tc was achieved with high detection efficiencies of 60.72 ± 1.93% and 72.83 ± 0.81% for resin with TEA and MDOA functional groups, respectively. The detection limit was determined to be less than the maximum contaminant level (33 Bq L-1) established under the Safe Drinking Water Act. The two functionalized resins were demonstrated to be selective for pertechnetate from synthetic groundwater containing up to 1000 ppm Cl-, SO42-, and HCO3- and up to 1200 ppb Cr2O72- in an acidic medium. [ABSTRACT FROM AUTHOR]