Process technology for extraction of uranium from seawater has been initiated in India on bench scale field trials and for this purpose special adsorbents have been synthesised by radiation grafting technique. These adsorbents are in the form of leaflets that provide efficient contact patterns with water body in the sea. However, it was observed that during the extraction of uranium from seawater/brine, a few transition elements like vanadium also got extracted by the adsorbents. The product elute solutions were then stored in large glass-lined mild steel tanks, which lead to the extraction of iron from the tanks into the solutions. The main challenge was to separate uranium from these transition elements and then estimate its concentration by laser fluorimetry (LF). This paper reports the radiochemical separation procedure standardised for determining the concentrations of uranium metal ions from lean solutions of seawater/brine and its estimation by LF.