Minor contamination of transition metals (TM) in Si ruins the performance of the electronic devices by forming several well-known recombination centers. Immense care should therefore be taken, that all processing steps in device fabrication are free of TM contaminants. Based on two well-studied Cu and Ni defects in Si, we propose a novel, fast and cost-effective electrical method to quantify wafer bulk contamination with Cu and Ni impurities from alkaline silica solutions used in chemical–mechanical polishing (CMP). Monitor wafers to test the CMP process are pre-irradiated with high-energy electrons to create a uniform concentration of radiation defects. Mobile copper and nickel species, introduced by the polishing into the wafer are captured by specific electrically active radiation defects, that can be detected using deep-level transient spectroscopy (DLTS). The optimal irradiation fluence for achieving the best sensitivity is shown to be rather low, leading to only ∼ 10% compensation of the initial wafer conductivity, thus ensuring DLTS applicability. We compare the experimentally measured deep-level depth profiles with simulated ones and establish a potential detection limit of the method, which is as low as 10⁸ cm⁻². Our proposed detection technique can be used in more generality to evaluate the potential danger of low bulk contamination from different processing treatments of the Si surface.