Abstract A simple method for the simultaneous estimation of plasma volume, extracellular fluid volume, total body sodium, and total body potassium is described. Its use provides important advantages in both clinical and investigative medicine. The procedure utilizes T-1824, Br 82 , Na 22 , and K 42 , Evans blue dye is determined spectrophotometrically. Radiobromide is separated chemically by use of a simple ion exchange column containing Amberlite IRA-400. The remaining mixture of Na 22 and K 42 is delineated by short-term differential decay counting. Data are presented which demonstrate that this method gives results which agree with published values for normals obtained by other methods. In addition, when dietary sodium intake is altered, the volumes of distribution of bromide ion change in the expected directions.