A study has been made of the substances excreted in the urine after the administration of butyl 4-hydroxy-3:5-diiodobenzoate (BHDB) to man, rabbits and rats. 2. The principal excretory products found in the urine of seven patients with thyrotoxicosis, two patients with myxoedema under treatment with thyroxine, and one normal volunteer were 4hydroxy-3:5-diiodobenzoic acid and its methyl ether. These two acids accounted for 90 % or more of the total urinary iodine. Less than 2% of the urinary iodine consisted of iodide. 3. The excretion of the methoxy acid appeared to be greater in patients with thyrotoxicosis than in other subjects studied. The implicatioris of this observation in relation to processes of biological methylation are discussed. 4. In rabbits and rats treated with BHDB, only the hydroxy acid was isolated from the urine.