Estrone-6,7-3H-sulfate-35S was injected into a woman with a bile fistula and parallel collections of bile and urine were made for 47 hr. The excretion of 3H amounted to 67% in the urine and 33% in the bile, whereas the corresponding values for 35S were 64 and 3%. Metabolites were separated according to conjugate types by chromatography on alumina and Celite. Estrone sulfate (E1-S) and estriol-3-sulfate (E3-3S) were analyzed as such by reverse isotope dilution with particular emphasis placed on the changing nature of the 35S/3H ratios with time. Other conjugates were assayed by hydrolyzing with appropriate enzymes followed by purification of the estrogens, usually by column chromatography and isotope dilution techniques. In the early stages the 35S/3H ratios of E1-S in the urine and bile were similar to that injected; then they decreased rapidly. The corresponding ratios for E3-3S in urine were lower. The sulfates comprised similar percentages of the respective fluids. However, there were qualitative differences. E3-3S, with lesser amounts of E1-S, predominated in the urine, whereas sulfates of E1, ring D α-ketols, 15α-hydroxyestrone (15α-OHEi) and 15α-hydroxyestradiol (15α-OHE2) were found in comparable amounts in the bile. Glucosiduronates were more concentrated in the urine than in the bile. The major glucosiduronates of the 0–3 hr urine were that of E3, 2-hydroxyestrone, 16-epiestriol (16-epiE3) and E1- Glucosiduronates of E3, E1 and 2-methoxyestrone predominated in the bile. Sulfoglucosiduronates as a class were higher in the bile than in the urine. Those identified, including the sulfoglucosiduronates of E3, 16-epiE3, 16α-hydroxyestrone and 16β-hydroxyestrone, were found in comparable amounts. New estrogen double conjugates were found in significant amounts (24%) in the bile. These were the sulfo-N-acetylglucosaminides of 15α-OHEi and 15α-OHE2. In addition, the latter comprised about 1 % of the urinary radioactivity. Finally, a number of conjugates were found which were classified as “polar” unidentified by the criteria of chromatographic elution pattern, high voltage paper electrophoresis and enzyme hydrolysis. Some of these appeared to be double conjugates.