The report describes the measurement of urinary organic halogen compounds. The method is an application of the adsorbable organic halogen assay which is widely used for the analysis of industrial waste water and drinking water. It was found that this assay can be applied to human urine if the urine is pretreated to hydrolyze the mucins so as to cleave the neuraminic acid residues responsible for the high viscosity of these slimy proteins. The method was found to be sensitive down to 1 microgram of organic halogen/100 ml of urine. Fifty to 260 micrograms of organic halogen was measured in the night urine of healthy, occupationally unexposed volunteers. Since many toxic chemicals to which man may be exposed environmentally or occupationally are, in fact, halogen compounds, this assay may be used to monitor for human exposure.