The determination of copper and manganese in biological materials and river waters by sequential metal vapor elution analysis (SMVEA) using an atomic absorption detector (AA) is reported. An improved molybdenum column (open column, i.d. 1.22 mm) with three ring supporters was developed for SMVEA. An optimum flow rate of carrier gas (pure argon) for separation of metal vapors was 4.0 ml min(-1). Copper and manganese peaks separated from Al, Ca, Cd, Fe, K, Mg, Na, Pb, and Zn peaks at a vaporization temperature of 1950 degrees C and a column temperature of 1900 degrees C. The appearing order of these metals was Cd, Zn, Pb, Cu, Na and Mn. It was understood by considering the boiling points of these metals or chlorides. The delay of appearing time is due to an interaction between the metal vapors and inside surface of the column. Under the experimental conditions, the number of theoretical plates was 11.3 for Cd, 89.6 for Cu, 160 for Na, and 258 for Mn in the improved column. Under the optimal experimental conditions, NIST biological standards and river waters were analyzed for copper and manganese. The analytical results agreed well with the certified values and the recoveries were in the range of 94 to 109%. By SMVEA, it was found that copper and manganese in biological materials and waters were determined without interference of matrix elements, after only acid digestion for biological materials and no chemical treatment for river water samples.