The beneficial effects of fluoride are well known, but higher levels are dangerous to health. Existing remediation methods used to address the latter situation all have limitations. This experiment explores the underlying fundamentals of an alternative defluoridation technology based on redox-driven ion exchange, here into polyaniline films. The proposed measurements include static observations of fluoride distribution at different stages of uptake from NaF and ejection into HClO4; based on nanogravimetric data, solvation state changes are also predicted. The experiment then extends to dynamic observations of uptake and ejection using event mode acquisition during slow scan voltammetric scans. Contrast between polymer and solvent will be achieved using d5-aniline. The outcomes are relevant to design of materials and devices for production of drinking water in remote locations.