Fluorescence spectroscopy offers several advantages over other methods of detection and quantitation of chemical compounds. This technique has been underutilized in detection and quantitation of herbicides. The fluorescence properties of 39 herbicides representing several major types of chemistry were determined. The fluorescence of analytical standards was measured in acetonitrile, acetonitrile + water, and acetonitrile + water + strong acid. Fourteen of the 39 herbicides fluoresced to some extent, and seven (bentazon, chloramben, difenzoquat, fluometuron, imazaquin, MCPA, and norflurazon) were identified as good candidates for further method development. The technical advantages and disadvantages of fluorescence spectroscopy of herbicides are discussed.