1. (3)H-labelled o-aminoazotoluene was synthesized from [G-(3)H]o-toluidine on a semi-micro scale. 2. An association of (3)H with DNA, RNA and protein from the liver, kidney and spleen of female C57b mice was demonstrated after the administration of a single dose of [(3)H]o-aminoazotoluene. 3. This association is judged to represent covalent binding as a result of experiments involving solvent extraction, examination of the acid hydrolysates of the DNA and RNA and administration of [(3)H]water with unlabelled o-aminoazotoluene. 4. Examination of the extents of binding at various times after the administration of a single dose of [(3)H]o-aminoazotoluene showed that there was a peak of binding to liver DNA in the female mice at about 16hr. that was not present in the male mice. 5. The extent of binding to DNA, RNA and protein at 16hr. in the female C57b mouse liver was greater than that in the spleen and kidney.