Sodium tetraphenylborate (NaTPB) can be used to recover trace amounts of ammonium and cesium ions from aqueous wastestream simulants. The cesium or ammonium salts precipitated by mixing aqueous NaTPB with the waste stream are dissolved in acetone. In the case of ammonia, the pH is increased by addition of NaOH(aq). The resulting solution, containing a much higher concentration of ammonia than the original waste stream, is then distilled to recover both ammonia and acetone. In the case of cesium, the TPB anion is precipitated by addition of tripropylamine and HCl, and the Cs cation is isolated as CsCl. Subsequent treatment with base Liberates tripropylamine and leaves an aqueous solution of NaTPB. In either case, the regenerated NaTPB can then be recycled back into the waste stream. Recovery of cations was quantitative for ammonium and 90% for cesium. Recovery of TPB was quantitative within experimental error. Process designs based on the iterative batch methods are proposed to allow continuous-flow recovery of the products from aqueous waste streams. The conversion of CsTPB to CsCl, with recovery of the TPB anion, may help to avoid problems associated with radiolysis of TPB by radioactive Cs cations.