Preparative, extraction, and analytical methods for simultaneous determination of legacy and insensitive munition (IM) constituents in aqueous, soil or sediment, and tissue matrices

Abstract

No standard method exists for determining levels of insensitive munition (IM) compounds in environmental matrices. This project resulted in new methods of extraction, analytical separation and quantitation of 17 legacy and 7 IM compounds, daughter products of IM, and other munition compounds absent from USEPA Method 8330B. Extraction methods were developed for aqueous (direct-injection and solid-phase extraction [SPE]), soil, sediment, and tissue samples using laboratory-spiked samples. Aqueous methods were tested on 5 water sources, with 23 of 24 compounds recovered within DoD QSM Ver5.2 limits. New solvent extraction (SE) methods enabled recovery of all 24 compounds from 6 soils within QSM limits, and a majority of the 24 compounds were recovered at acceptable levels from 4 tissues types. A modified chromatographic treatment method removed analytical interferences from tissue extracts. Two orthogonal high-performance liquid chromatography-ultraviolet (HPLC-UV) separation methods, along with an HPLC–mass spectrometric (HPLC-MS) method, were developed. Implementing these new methods should reduce labor and supply costs by approximately 50%, requiring a single extraction and sample preparation, and 2 analyses rather than 4. These new methods will support environmental monitoring of IM and facilitate execution of risk-related studies to determine long-term effects of IM compounds.