Validation and standardization of SPE and HPLC-UV methods for simultaneous determination of legacy and insensitive munitions

Abstract

There have been few attempts to consolidate legacy and insensitive munitions analyses. Furthermore, there are no standard methods for insensitive munitions (IM) in tissues, resulting in overlapping methods and supplementary analyses. The goal of the present study was to validate extraction and instrumental methods previously developed and address analytical methodology gaps (missing tissue matrices, combined legacy and IM analysis, and IM compounds). The method encompasses analytes in waters, soils, and tissues. The primary and secondary instrumental methodologies use high performance liquid chromatography-ultraviolet (HPLC-UV) and an alternate LC-mass spectrometry (MS) method, which includes 26 compounds of interest (legacy munitions, IM, IM degradation products, and other munitions compounds). The methods were formally evaluated during a series of double-blind round robin studies including a broad variety of laboratories (Government Department of Defense (DoD), Government non-DoD, ammunition manufacturing, commercial, and academic). The results of these round robin studies were gathered to generate recovery ranges for each of the 26 compounds in each of the matrices. The recovery ranges were subsequently compared with existing recovery ranges for standard explosives analysis, United States Environmental Protection Agency (USEPA) 8330B. The validation study reveals a capable method, which reduces analysis time for IM and legacy munitions analyses.