In a previous contribution, a new application of the polymersurfactant aggregate (PSA) process was developed; the removal of metallic anions from dilute aqueous solutions. A subsequent pH adjustment method has been developed to recover the metallic anions from the flocculated PSAs into a concentrated solution and then to recover the polymer (PAA) and surfactant (MTAB) for recycling. A base solution is firstly added to the flocs to leach out the bound metallic anions in 15 minutes, and then a coarse filter is used to separate out the basic solution containing 5-20 times more concentrated metallic anions than the original effluent. The flocs can then be completely dissolved in an acid solution for recycling. The results show that the recovery efficiency of CrO42-at an optimum pH of 12 is 94%, and the recovery efficiency of PAA-MTAB at its optimum pH of 1.4 is 94%. The removal efficiency of 0.2 mM CrO42solution remains at the same level using recovered PAA-MTAB. In short, the sequential pH adjustment method is able to recover and concentrate the metallic anions from the flocculated PSAs, and then recover the removal agent for recycling into the process with little deterioration of removal ability.