Several secondary cleanup procedures have been tested for hydrolytically and radiolytically degraded TRUEX process solvent (0.2 M. n-octyl(phenyl)N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO)-1.2 M tributylphosphate (TBP) in n-dodecane). Sodium carbonate scrub was used as primary cleanup. For the secondary cleanup macroporous anion exchange resins and other solid adsorbents, such as goethite (a-FeOOH), alumina and activated charcoal were used. The effectiveness of a cleanup procedure was established by its capability to restore the original americium(III) distribution ratio from low HNO3concentration, that is characteristic of pristine process solvent. Further information was obtained from the measurement of up to seven successive AmfJIT) distribution ratios with the regenerated solvent, using the stripping conditions of the TRUEX process. Although all the procedures tested proved to be effective in removing most of the unwanted acidic products from the degraded solvent, the use of a strong base macroporous anion exchange resin, acid washed activated charcoal and acid washed alumina were particularly successful.