<p>A simple titrimetric method for sequential determination of free acidity and uranium (U) concentration in the same sample aliquot of process stream solution from uranium extraction plant (UEP) of UO₂ production facility is described in the present paper. The method is valid for both aqueous and organic process stream solutions received from UEP. In the present paper, two methods namely Method-A (with complexant) and Method-B (without complexant) have been described. In Method-A, potassium oxalate is used as complexant and NaOH as titrant. Where-as in Method-B, titration is performed without using any complexing agent and Na₂CO₃ is used as titrant. The uranium values obtained from both the methods have been compared with that of Davies &amp; Gray method and Gamma Ray Spectrometric method and found to be in good agreement. The developed method can be applied to solutions containing 7–650&#xa0;g/L of uranium covering all the aqueous and organic process stream solutions except uranyl nitrate raffinate with a precision of better than 5% RSD.</p>