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1. The preparation of tanned gelatin spheres and granules from high-molecular-weight gelatin is described. This material is comparatively hard, giving high flow rates, is insoluble in water at temperatures between 0° and 100° and is resistant to digestion by trypsin and chymotrypsin. The high-molecular-weight fraction of gelatin was prepared by precipitation with polyethylene glycol, and the spheres and granules prepared from this fraction were hardened and insolubilized by tanning with either formalin or chromium salts or both. 2. The spheres and granules were used successfully for the separation of protein molecules and other protein-aceous materials ranging in molecular weight from 200 to greater than 6000000. This gel exclusion material has several properties superior to those of other products used for similar purposes. Further, it was noticed that the porosity of the spheres differed considerably from that of the granules.