Radiostrontium is concentrated in the shells of mollusks and other animals due to the isomorphic substitution of strontium for calcium in the calcium carbonate shell matrix. Radiochemical separation of strontium from such matrices is difficult because of the chemical similarity between strontium and calcium. This paper describes a technique using a commerically-available, solid-phase extractant to separate Sr-89 and Sr-90 from high concentrations of Ca2+. The extractant removes Sr(NO3)2 from acidic nitrate media, and strontium activities are determined via conventional β-counting techniques. This method has been used to process mollusk shells collected from contaminated reactor cooling ponds at the Savannah River Site and Chernobyl Nuclear Power Plant.