Abstract.A procedure for the determination of ammonium is described, based on its transformation into ammonia gas and subsequent measurement by UVvisible molecular absorption spectrometry at 194 nm. Two different procedures for generating the ammonia are proposed, using NaOH solution and solid NaOH, respectively. After generation conditions for both procedures had been optimized, better sensitivity was observed with solid NaOH. In these conditions, the method showed two ranges of linear response: from 1 to 100/~g and from 100 to 400 #g of ammonium. Finally, we determined ammonium in wine samples. Preliminary studies indicated that the only observable interfering species was ethanol, which could be eliminated by subjecting the sample to vacuum evaporation until nearly dry. This process also increased the sensitivity of the method by as much as ten times. The values obtained from three different wine samples yielded results within the range of the concentration obtained by other authors. The recovery of ammonium added to the wine samples was around 95%.