A method involving ion-exchange chromatography and titration was developed. A diluted sample was run through a cation-exchange resin column. After the eluate was boiled, it was titrated with 0.02NNaOH to find the sodium citrate content (Titration I). An equal volume of the diluted sample was eluted through an anion-exchange resin column and the eluate was titrated with 0.02NHCl to assay for total sodium bicarbonate and sodium citrate (Titration II). Subtracting the result of Titration I from that of Titration II, gave the sodium bicarbonate content. The cation-exchange chromatography step was validated previously. The anion-exchange chromatography step was validated by assaying pure sodium bicarbonate and sodium citrate separately. The overall percent recoveries (+ SD) were 98.9+0.2% for sodium citrate and 98.1+0.1% for sodium bicarbonate (n = 3). Average percent recoveries (+SD) from synthetic mixtures of the two salts were (n = 4): 99.3+0.5% for sodium citrate and 98.0+1.2% for sodium bicarbonate. The method was applied to commercially available formulations.