Abstract: Kinetics of the radiolysis of the type 732 polystyrene sulfonic acid resin has been investigated.While comparing radical concentration determined by ESR method with amounts of SO42- obtained after irradiation of the 732-resin, we have found that the resin contains two different structures. One form is so-called normal sulfonic acid resin (i. e. o, p-substituted). The other form is tertiary substituted sulfonic acid resin which was reported as m-substituted earlier. The radiolysis of the dry resins obeys first order kinetics, and Kd for dry tertiary substituted sulfonic acid resin equals to 1.24×10-7 rad-1. Its content approximately amounts to 0.2%. The Kd of dry normal resin equals to 4×10-11 rad-1, G = 0. 199.The life time of the radicals of the resin is very long. It can be quenched by water or annealing. In comparison with the original resin, the concentration of radicals of the dry resin which has been pre-irradiated and quenched with water markedly increased under y-radiation.when wet resin was irradiated, the yield of SO42- increased. The kinetic equation of radiolytic hydrolysis has been derived. The Gso42- value calculated with the energy absorbed by water is equal to 8.0±0.2, 1GS042- of unstable resin = 5.3±0.2 and 2Gso42- of stable resin =2.66. Possibly Gso42- is equivalent to GH2o*.