The new metrology, Advanced Poly-silicon Ultra-Trace Profiling (APUTP), was developed for measuring bulk Cu and Ni in heavily boron-doped silicon wafers. A Ni recovery yield of 98.8% and a Cu recovery yield of 96.0% were achieved by optimizing the vapor phase etching and the wafer surface scanning conditions, following capture of Cu and Ni by the poly-silicon layer. A lower limit of detection (LOD) than previous techniques could be achieved using the mixture vapor etching method. This method can be used to indicate the amount of Cu and Ni resulting from bulk contamination in heavily boron-doped silicon wafers during wafer manufacturing. It was found that a higher degree of bulk Ni contamination arose during alkaline etching of heavily boron-doped silicon wafers compared with lightly boron-doped silicon wafers. In addition, it was proven that bulk Cu contamination was easily introduced in the heavily boron-doped silicon wafer by polishing the wafer with a slurry containing Cu in the presence of amine additives.