IgD has been isolated in homogeneous form from a dysgammaglobulinemic plasma. This preparation of IgD represents the first pure preparation isolated from a plasma having a titer of IgD approaching that of normal plasma rather than from a plasma having a high titer such as myeloma plasma. The isolation procedure was developed from the solubility properties of IgD in solutions of (NH 4) 2SO 4, Zn-acetate, Rivanol, etc. Final purification involved gel filtration on Sephadex G-200, batch adsorption on DEAE Sephadex A-50, chromatography on DE-52 microgranular cellulose, and immunoadsorption. The procedure permitted the isolation of IgD from large volumes of plasma and yielded enriched fractions of albumin, IgM and IgG. The physicochemical properties of IgD were determined. The electrophoretic mobility in veronal buffer, pH 8.6, Γ/2-0.1 was 2.52 × 10 −5 cm 2/V sec. The isoelectric point determined by electrophoresis in phosphate buffers, Γ/2-0.1 was 5.85. The sedimentation coefficient extrapolated to zero concentration in water was 6.92S. Molecular weight by osmotic pressure was 183,000, by sedimentation equilibrium was 178,800, and by a combination of sedimentation, viscosity, and partial specific volume data was from 128,500 to 175,700. The weight intrinsic viscosity was 0.094, and the partial specific volume was 0.717. Molecular dimensions were calculated by assuming prolate and oblate ellipsoids of revolution. The IgD was homogeneous by electrophoresis, sedimentation and by antigenicity.