Accurate quantitation of 1,3,5‐triamino‐2,4,6‐trinitrobenzene (TATB) is important because of its strategic use as an energetic material. A purity determination is also needed for the proper assessment of performance. A fast and sensitive method has been developed to measure the purity of TATB in polymer‐bonded materials. The target material is extracted with DMSO, and the extract is separated on a reversed‐phase chromatography column. The column effluent is monitored by diode array detection (DAD) at 354 nm. The characteristic UV‐Vis response and retention time identify the individual components when compared to pure compound standards. The chemical structures of compounds with no pure standards available have been determined by high‐resolution mass spectrometry (MS) and MS/MS. The major component, TATB, along with 1‐chloro‐3,5‐dinitro‐2,4,6‐triaminobenzene (T4A) and mono‐benzofuroxan (FX1) were quantitated directly from pure compound standards. Several trace concentration components, mono‐benzofurazan (F1), 1‐bromo‐3,5‐dinitro‐2,4,6‐triaminobenzene (Br‐T4A), 2,4,6‐triamino‐1‐nitroso‐3,5‐dinitrobenzene (MN‐TATB), 2,4,6‐triamino‐1‐hydroxyl‐3,5‐dinitrobenzene (HO‐TATB), and 2,4,6‐triamino‐1‐nitrile‐3,5‐dinitrobenzene (Nitrile‐TATB) were also detected and structures verified via MS/MS. Approximate concentrations were determined using calibrations from standards of similar structures. Additional trace components were also detected by MS. Contained herein are the results of analyses of TATB‐based materials characterized for polymer‐bonded formulations compared to different preparations of TATB. The accuracy, details, and process of developing this method are reported here.