Microbore liquid chromatography and positive ion electrospray mass spectrometry are applied to the determination of 16 carbamate, urea, and thiourea pesticides and herbicides in water. The electrospray mass spectra of the analytes were measured and are discussed and mobile-phase matrix effects were evaluated. Analyte positive ion abundances are generally inversely related to the concentration of acetic acid in the acetonitrile-water mobile phase in the range of 0.001-0.1% (v/v) acetic acid. Using an internal standard for quantitative analyses and no acid in the mobile phase, retention time precision, peak width precision, concentration measurement precision, mean recoveries, and instrument detection limits were determined in reagent water. The 16 analytes were also measured in fortified environmental water samples from a recreational lake, a groundwater well, a cistern, a farm pond, and drinking water. These measurements were at 5 ng/mL of each analyte, which is within the range expected for environmental pesticide and herbicide contaminants. The analytes were separated from the environmental water matrixes with an on-line extraction and concentration to provide rapid sample analyses without a slow off-line liquid-liquid or liquid-solid-liquid extraction and extract concentration. Recoveries of 12 of the analytes from 4 environmental water samples were in the range of 75-124% with relative standard deviations in the range of 11-16%.