The present study aims at the generation of a triblock copolymer vs sodium sulfate aqueous biphasic system (ABS), its application toward extraction of molybdenum species, and finally purification and regeneration of the block copolymer. The ABS was characterized for its biphasic region by constructing the phase diagram using turbidometric titration methods. Extractions were monitored using the spectrophotometric method directly in the block copolymer medium. Complete extraction of molybdenum species was observed in this method. Interference from other closely related metal ions in the extraction process was found to be negligible excepting oxo and polyoxometallates of vanadium and tungsten. Regeneration of the polymer was done using a thermoseparation technique followed by successive treatment with ion exchange resins. similar to 87% of the pure triblock copolymer could be regenerated as a result of such treatment.