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The stable isotope analysis of black powder is of utmost significance with regard to its further comparison and traceability in explosion-related cases. To date, only a limited number of studies have reported the stable isotope analysis of black powder using isotope ratio mass spectrometry (IRMS). However, because the sulfur content in black powder is high, sulfur deposition is extremely likely during the analysis process, thereby damaging the instrument and affecting the reproducibility of the results. Therefore, desulfurization of black powder samples prior to IRMS analysis is extremely desirable. Desulfurization and stable isotope analysis were performed on 12 black powder samples obtained from cases that happened in eight different areas in China, and the carbon, nitrogen, and oxygen isotope ratios in all the samples were effectively distinguished.