Electrochemical Detection of Vanadium Using a Boron‐Doped Diamond Electrode as a Surrogate for Radioactive Heavy Metals

The release of radioactive heavy metals from radioisotope research laboratories necessitates rapid and on‐site analytical methods that complement conventional techniques such as inductively coupled plasma mass spectrometry (ICP‐MS) and accelerator mass spectrometry (AMS). In this study, a sensitive electrochemical detection method based on a boron‐doped diamond (BDD) electrode was developed in nitric acid media. Because experiments involving radioactive nuclides require specialized facilities, vanadium was employed as a nonradioactive surrogate to optimize anodic stripping voltammetry (ASV) conditions. Systematic optimization of experimental parameters, including electrolyte composition, electrode material, surface termination, and voltammetric method, identified ASV using an O‐terminated BDD electrode as the most effective approach. Under optimized conditions (deposition potential of −1.2 V [vs. Ag/AgCl] and deposition time of 180 s in 0.5 M HNO ₃ ), a limit of detection (LOD) of 0.478 μM was achieved, outperforming CV, DPV, and SWV. Interference studies revealed that Ru(III) and Ce(III) significantly affect the vanadium signal but can be effectively mitigated by pH‐controlled precipitation and phosphoric acid addition, respectively. In contrast, Pd(II) interference remained unresolved due to its dominant electrochemical response. Finally, the applicability of the developed method to actinide‐relevant systems was demonstrated using a ²³⁷ Np solution, which exhibited a characteristic anodic signal at ~1.7 V (vs. Ag/AgCl), comparable to that of vanadium. These results highlight the potential of BDD‐based ASV for monitoring radioactive heavy metals in nitric‐acid environments.