The effects of pH on the speciation of some tributyltin and triphenyltin compounds in spiked sediments from the Anacostia River were studied. The compounds included tributyltin chloride, oxide, and acetate as well as triphenyltin chloride, hydroxide, and acetate. Mo¨ssbauer spectroscopy was used to measure the speciation of the triorganotin compounds in the spiked sediments. In general, for the three pHs (5, 7, and 9) studied, the Mo¨ssbauer parameters, quadrupole splitting, and isomer shift, varied depending upon the sediment site and the pH. The r-values (ratio of quadrupole splitting to isomer shift), which indicate the co-ordination of the tin atom, were greater than 2.1 in all cases, indicating that the co-ordination around the tin atoms in all the spiked sediments is greater than four. The variation in the Mo¨ssbauer parameters with pH at different sites in the Anacostia River reflects the variation in the components of the sediments.