Trace analysis of explosives in soil: pressurized fluid extraction and gas and liquid chromatography-mass spectrometry

Soil samples are collected from the former Open Burn/Open Detonation Unit, Makua Military Reservation, on the island of Oahu, Hawaii. The soil is the Helemano series. The soil samples are fortified with eight explosives for development of the analytical method. These analytes are 2-amino-4,6-dinitrotoluene; 1,3-dinitrobenzene; 2,4-dinitrotoluene (DNT); hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX); nitrobenzene (NB); octogen; 1,3,5-trinitrobenzene; and 2,4,6-trinitrotoluene. The analytes are recovered with pressurized fluid extraction and measured with liquid chromatography (LC), LC-mass spectrometry (MS), and gas chromatography-MS. Average recoveries of the seven analytes, except for NB, range from 67% to 110% from freshly fortified samples. The procedure fails to extract NB in soil. The average recoveries decrease from 67-110% to 41-81% as the soil is aged for 1 day to 6 months after fortification of the soil with the seven explosives. The field samples are analyzed for the presence of explosives, of which DNT and RDX are indeed detected. The results obtained with this procedure agree well with those obtained by an independent laboratory following the standard U.S. Environmental Protection Agency (EPA) method SW-846 8330. Compared with the EPA method, this new method provides MS confirmation of the analytes, and the extraction requires approximately 15 min, rather than 18 h by the EPA method.