A technique for the analysis of aldicarb and two of Its degradation products Is described. The use of a short capillary column coupled to a mass spectrometer Is found to facilitate the analysis of the thermally labile carbamate pesticide. Methane and Isobutane chemical Ionization reagent gases are evaluated. The limits of detection for aldicarb, aldicarb oxime, and aldicarb nitrile are 0.3 ng, 1.2 ng, and 0.15 ng, respectively. Application of the technique to the study of the fate of aldicarb In anaerobic groundwaters Is described. Aldicarb Is found to slowly hydrolyze to aldicarb oxime In sterile anaerobic groundwater at pH 8.2; In the presence of a high concentration of anaerobic microorganisms, however, aldicarb rapidly degrades to aldicarb nitrile.