The use of spectrofluorimetry to determine the fluorescent derivative of the insecticide promecarb, following hydrolysis to the corresponding phenol in basic media and subsequent coupling with the labelling agent dansyl chloride, is described and discussed. A study of media of different basicity and of different temperatures for both reactions gave optimum conditions of 20 min for the hydrolysis reaction and 10 min for the labelling reaction at 55 degrees C in 0.05 mol dm-3 sodium hydrogen carbonate solution with a reagent to insecticide ratio of 12:1. The effect of the solvent on the formation of the dansyl derivative and on the extraction process was studied using nine and seven solvents, respectively. The use of a mixture of acetone and water (50 + 50, v/v) and an extraction into cyclohexane gave the best results. The minimum detectable concentration of promecarb in the experimental assays was 100 ng ml-1. The error and relative standard deviation at a concentration level of 0.6 micrograms ml-1 were 9.7 and 10.9%, respectively. Air samples containing promecarb at different concentration levels were analysed.