A sensitive method was developed for the determination of ammonium in an aqueous solution based on gas phase light scattering. In a stream of carrier gas, the gaseous ammonia from the alkalized solution formed a volatile ammonium chloride derivative by reacting with gaseous hydrogen chloride; the gaseous ammonium chloride was analyzed by nondispersive atomic fluorescence spectrometry. The mechanisms of the method are elucidated based on evaporative light scattering detection. Parameters such as temperature, amount of sodium hydroxide, and carrier gas flow rate were studied. Under optimal conditions, the detection limit of ammonium-nitrogen was 0.045 μg. The method was successfully applied to the determination of ammonium in certified reference materials, and tap and seawater samples.