At the U.S. Department of Energy's Savannah River Site (SRS), the In-Tank Precipitation (ITP) process uses sodium tetraphenylborate (TPB) to decontaminate soluble High Level Waste (HLW) by precipitating radioactive cesium-137. However, palladium, and possibly other metals that are present in HLW stored at the SRS, are suspected of catalyzing the degradation of the TPB . Testing demonstrated that the present system configuration could not cost-effectively meet the safety and production requirements in the presence of the decomposition reaction. A more fundamental understanding of the mechanism of catalytic degradation of TPB is required to provide a sound technical basis for the Small Tank TPB Precipitation Process proposed as an alternative to ITP. The work described herein was undertaken under Technical Task Plan (TTP) ORNL/CF 99/7 1, entitled Technical Task Plan for Investigating the Mechanism of Catalytic Tetraphenylborate Decomposition Using Nuclear Magnetic Resonance Spectrometry. The objective of this project was to use, to the extent possible, Nuclear Magnetic Resonance (NMR) spectrometry as an analytical method to gain more insight into the kinetics and degradation mechanism of TPB.