The optimum conditions for the regeneration of strong base anion exchange resins of type-I and type-II were determined for cost - effective separation of isotopes of boron by ion exchange chromatography. The possibility of using unspent alkali content of the effluent was also exploited Removal of carbonate impurity from Rayon grade caustic lye (used as regenerant after dilution) and recycling of Ba(OH)(2) was studied to avoid waste disposal problems. The determination of (i) ion exchange capacity of Duolite-162 resin for hydroxyl -chloride and hydroxyl - borate exchanges, (ii) isotopic exchange separation factor by batch method and (iii) effect of concentration of boric acid (in presence and absence of mannitol) on isotopic exchange separation factor to test the suitability of the type-II resin for this process are discussed.