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Five alcoholics administered 1 g of disulfiram in soybean emulsion by deep intramuscular injection were found to have insignificant urinary levels of disulfiram metabolites compared with five patients on oral disulfiram. Disulfiram administered in this way is unlikely to produce a significant reaction with ethanol, but its value as a placebo should not be discounted. In this pilot trial, the technique caused moderate local and systemic reactions and possible hepatic toxicity. Although in other respects the method is superior to surgical implants, modification of dosage and vehicle will be necessary, and the high incidence and severity of side effects preclude further clinical use of disulfiram in this form. Based on the work of Gordis and Peterson, a qualitative and quantitative thin-layer chromatographic urine assay method for the disulfiram metabolite diethylamine, measured as cupric diethyldithiocarbamate, was developed. This is practicable in a hospital laboratory situation and has application for compliance testing in patients on oral disulfiram.