A method is presented for the identification and determination of explosives and other related compounds possessing thermally labile nitro or nitroxy groups. It involves the use of high performance liquid chromatography (HPLC) with a nitrosylspecific detector (TEA Analyzer). Results are presented for EGDN (ethanediol dinitrate), NG (glycerol trlnitrate), PETN (2,2-bis( nitroxymethyl)-l,3-propanediol-l,3-dinitrate), Petrin (2-hydroxymethyl-2-nitroxymethyl-l,3-propanediol-l,3-dinitrate), PEDN (2,2-bis( hydroxymethyl)-l,3-propanediol-l,3-dinitrate), RDX (hexahydro-l,3,5-trinitro-s-triazine), NGu (1-nitroguanidine) and HMX (octahydro-l,3,5,7-tetranitro-1,3,5,74etrazocine). Calibration curves covering a concentration range of three orders of magnitude are presented for RDX and PETN. The 90 YO confidence interval for quantiication of RDX is f1.6% at the 4-ng level and that for PETN is f3.2% at the 6-ng level. Retention behavior with silica and NH2-bonded phase HPLC columns is presented. Use of retention times on the two different columns coupled with a response on the nitrosyl-specific detector serves as a convenient method for identification. Although standard explosive preparations were analyzed at nanogram levels without purification, no interferences were presented by ancillary components such as plasticizers and stabilizers.Present techniques for the identification of small aniouiits of explosives usually involve the use of thin-layer chromatography (TLC) (1-3). Some improvements in speed and accuracy are possible through the use of spectrophotometric methods with the TLC techniques (4-6). Despite their widespread use, these techniques possess several disadvantages, including relatively large sample requirements that preclude their use for the analysis of trace quantities of explosive substances (3, 7).Recause of its speed, sensitivity, and simplicity, gas chromatography (GC) has also received attention as a method for the analysis of explosive preparations. This technique, however, is limited by the fact that many explosive compounds are incompatible with the usual GC conditions because of their inherent thermal instability and other problems (8-1 I).Satisfactory results have been obtained only for the analysis of thermally stable nitroaromatic compounds such as the nitro derivatives of toluene (12,13) and such ancillary constituents as plasticizers and stabilizers (9, 11, 14, 25).In an attempt to increase sensitivity and selectivity, GC has been employed with a variety of detectors. Limited success has been achieved using an electron capture detector (EC). However, great care must be taken to avoid overloading or contamination, and special techniques must be used to ensure linearity of response (12, lti, 17).Electron-impact mass spectrometry (MS) seemed to be advantageous for the analysis of explosives a t trace levels; but apart from its denionstrated potential for the identification of nitroarelies (It?), it shows little promise for the analysis of other types of explosives (19-21). Chemical ionization mass s...