The newly fielded insensitive high-explosive compound 3-nitro-1,2,4-triazol-5-one (NTO) is mobile in the environment due to its high water solubility and low affinity for soils. The weak acidity of NTO (pKa 3.67) presents a challenge to environmental analysis by high-performance liquid chromatography but enables direct separation by ion chromatography (IC). Here we developed an IC method for NTO in natural water, soil, and postdetonation residue. A gradient potassium hydroxide separation effectively resolved the inorganic anions (F − , Cl − , NO2 − , Br − , SO4 2− , NO3 − , and PO4 3−) and NTO in 18 minutes. Suppressed conductivity of aqueous NTO was linear from 10 µg/L to 10 mg/L with a detection limit of 3 µg/L and quantitation limit of 9 µg/L. Recoveries of NTO-spiked natural water samples were 93%-118% at concentrations of 30, 100, and 500 µg/L. Recoveries of NTO-spiked soil samples were 91%-114% using deionized water (DI) extraction. NTO was completely recovered with DI-extraction in two postdetonation residue samples of IMX-101 but only partially recovered (58% and 69%) in two higher-concentration residues, potentially due to incomplete dissolution of the energetic particle matrix. These results support IC for confirmation analysis of environmental samples and for screening natural water samples while simultaneously analyzing inorganic ions. DISCLAIMER: The contents of this report are not to be used for advertising, publication, or promotional purposes. Citation of trade names does not constitute an official endorsement or approval of the use of such commercial products. All product names and trademarks cited are the property of their respective owners. The findings of this report are not to be construed as an official Department of the Army position unless so designated by other authorized documents.