Analysis of uranium in U and Pu fuel samples was carried out by the modified Davis and Gray method. Sorption of Pu from analytic waste solution was studied by using macroporous bifunctional phosphinic acid (MPBPA) resin. The batch distribution data showed that the addition of nitric acid resulted in higher distribution values for plutonium. Column studies were carried out to determine the 10% breakthrough capacity of the resin for Pu(IV). The elution behavior of plutonium loaded on the resin was also studied