A tripodal framework bearing mixed donor sites was synthesized using simple reactions and was used for sensor applications in an aqueous medium by subjecting it to a nano-aggregate (N1) formation using a re-precipitation method. The characteristic fluorescence profile of the receptor due to the naphthyl moiety was observed. N1 showed selective recognition behaviour towards HSO4- in aqueous medium with a good linear range of 0-65 mu M. N1, the prepared nano-aggregates can be used to determine a lower concentration, as the detection limit for HSO4- ions in aqueous samples is 1.12 mu M in a wide pH range; thus, making them appropriate for the use in environmental or biological samples.