An extraction-anodic adsorptive stripping vol-tammetric procedure using microwave-assisted solvent extraction and a gold ultramicroelectrode was developed for determining the pesticide ametryn in soil samples. The method is based on the use of acetonitrile as extraction solvent and on controlled adsorptive accumulation of the herbicide at the potential of 0.50 V (vs. Ag/AgCl) in the presence of Britton-Robinson buffer (pH 3.3). Soil sample extracts were analysed directly after drying and redis-solution with the supporting electrolyte but without other pre-treatment. The limit of detection obtained for a 10 s collection time was 0.021 lg g -1. Recovery experi-ments for the global procedure, at the 0.500 lg g -1 level, gave satisfactory mean and standard deviation results which were comparable to those obtained by HPLC with UV detection.