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Triacetone triperoxide and hexamethylene triperoxide diamine are among the most used and most studied non-nitro based high explosives. Still, there are other peroxides which do not have reported methods for their detection. Direct Analysis in Real Time is an emerging ambient pressure ionization technique in mass spectrometry (MS). This contribution presents the analysis, characterization and detection of triacetone triperoxide (TATP) and hexamethylene triperoxide diamine (HMTD) using DART. Although typical experiments are done using helium, adding a small amount of ammonium hydroxide improved the detection limit to 30 ppb. This study also presents the detection and identification of benzoyl peroxide, tricyclopentanone triperoxide and tetramethylene diperoxide dicarbamide (TMDD) by MS and Raman microscopy. TATP showed a single peak at m/z 240.144 [M+NH4]+ with the peaks at m/z 223.118 [M+H]+ or 222.110 [M]+ completely absent. Deuterium enriched (TATP-d18) was analyzed for comparison. These presented a similar peak at m/z 258.267 [TATP-d18 +NH4]+. HMTD showed a peak at m/z 209.078 [M+H]+ and small adduct peak at m/z 226.103 [M+NH4]+ that allowed its detection in standard solution and lab made samples. TMDD showed several peaks with a base peak at m/z 101.033, molecular peak at m/z 237.081 [M+H]+ and a strong ammonium adduct at m/z 254.108 [M+NH4]+. All samples were analyzed by Raman Microscopy in order to characterize them and to confirm the MS results.