Procedures are presented for qualitative screening and subsequent quantitation of residues of explosives and related compounds found at sites contaminated by open burning/open detonation (OB/OD) disposal of munitions. Methods are reported for recovery of explosives and polycyclic aromatic hydrocarbons (PAHs) from soil via sonic extraction into acetonitrile; and explosives from water via trapping onto C18 disposable cartridges. Complimentary HPLC procedures were used for identification and quantification of these compounds. A qualitative HPLC gradient method was developed, and used to screen samples for a wide range of explosives and PAHs. Quantitation of explosives and their environmental reduction products was accomplished using HPLC isocratic methods. Recoveries of explosives and degradation products doped into sandy loam soil were greater than 90%. Corresponding recoveries from aqueous samples were comparable for the nitroaromatics, but were poorer for the nitramines. Criteria of detection for individual munition residues ranged from 0.067 mg 1−1to 0.37 mg 1−1.