High density serum lipoprotein underwent serologic and physicochemical alterations on aging during storage at 0°C. for 1 month, as judged by decrease of diffusion coefficient and increase of C' fixation. Ultracentrifugation, dialysis, and high concentrations of sodium chloride did not cause these changes. A protein sedimenting at density 1.24 in the ultracentrifuge reacted with antiserum to high density lipoprotein. Probably it was the protein portion of α lipoprotein dissociated from the lipide during ultracentrifugation. Although the antiserum to high density lipoprotein did not react with low density lipoprotein prepared from normal serum, it reacted with similarly prepared lipoproteins from the serum of a patient with biliary cirrhosis.