Accurate Urea Detection during Electrocatalytic Coreduction of CO ₂ and NO ₃ ^–

Urea synthesis through electrochemical coreduction of CO2 and nitrate offers a sustainable nitrogen fixation route. However, accurate quantification remains challenging due to nitrite interference. In this study, we develop a reliable approach for accurate urea quantification and denote it the Adaptive DAMO-TSC (A-DAMO) method, which introduces the nitrite concentration as a secondary calibration variable to eliminate false positives and improve accuracy across a broad range of urea concentrations. A full workflow and MATLAB code are provided to facilitate data processing. This study highlights significant problems of NMR-based urea quantification caused by H-bond acceptors such as nitrite. To validate A-DAMO in a practical application, synthesized and commercial ZnO were used as catalysts for electrochemical urea production. While conventional methods yielded misleading results, A-DAMO effectively corrected these inaccuracies, enabling an accurate and credible evaluation of urea synthesis performance.