Historically Sodium tetra-phenylborate (STPB) was used as a precipitating agent for potassium analysis in lab. It was only synthesized in labs in gram quantities and was never manufactured in large scale until late 80’s. In 90’s, we were interested to manufacture of STPB in Metric Ton quantities for ultimate usage for radioactive Cesium (Cs¹³⁷) precipitation from nuclear waste for business reasons. The presentation will give the overview of process scale-up problems for STPB. Root cause failures for making of the intermediate step and final product degradation mechanism due to presence of ‘3d’ transition metals will be discussed.