The preparation of pH-sensitive nanospheres by emulsion polymerization for the detection of trace levels of ammonia is described. A fluorescent, polymerizable xanthene dye was copolymerized with styrene, crosslinkers and further copolymers aimed at enhancing the sensitivity to obtain materials for sensing of ammonia. A half-seeded technique was used to obtain stable emulsions of the monomers which were cured to obtain nanospheres with covalently attached active components. The nanospheres were embedded in a silicon matrix and the sensor films obtained were investigated regarding their response to ammonia at concentrations between 25 and 1,000 ppb. Sensors containing polystyrene nanospheres crosslinked with divinylbenzene showed the best performance in ammonia measurements exhibiting detection limits (LODs) of less than 25 ppb ammonia.