24 Sep 2024

Validation of Sample Extraction and Analysis Techniques for Simultaneous Determination of Legacy and Insensitive Munitions (IM) Constituents

Abstract: Currently, no standardized method exists for the analysis of insensitive munitions (IM) in environmental matrices such as water, soils, and tis-sues. However, standardized methods, such as United States Environmental Protection Agency (EPA) 8330B, exist for legacy munitions for water and soil matrices. The lack of standardized methods for IM analysis leads researchers to use a wide variety of incomplete and overlapping analytical methodologies. The overall project’s first phase, Strategic Environmental Research and Development Program (SERDP) Environmental Restoration (ER)–2722, was to develop and optimize methods to address these methodological gaps by creating analytical methods for simultaneous analysis of IM and legacy munitions in water, soil, and tissue matrices. The main objective of the current project phase, Environmental Security Technology Certification Program (ESTCP) ER19-5078, is to build upon the previous work in phase one and to focus on the validation of the newly developed methods. Synergizing with the main objective of the overall project, the methods were validated and submitted to the EPA for inclusion as a possible addendum to EPA 8330B.

27 Sep 2021

Methods for Simultaneous Determination of 29 Legacy and Insensitive Munition (IM) Constituents in Aqueous, Soil-Sediment, and Tissue Matrices by High-Performance Liquid Chromatography (HPLC)

Abstract: Standard methods are in place for analysis of 17 legacy munitions compounds and one surrogate in water and soil matrices; however, several insensitive munition (IM) and degradation products are not part of these analytical procedures. This lack could lead to inaccurate determinations of munitions in environmental samples by either not measuring for IM compounds or using methods not designed for IM and other legacy compounds. This work seeks to continue expanding the list of target analytes currently included in the US Environmental Protection Agency (EPA) Method 8330B. This technical report presents three methods capable of detecting 29 legacy, IM, and degradation products in a single High Performance Liquid Chromatography (HPLC) method with either ultraviolet (UV)-visible absorbance detection or mass spectrometric detection. Procedures were developed from previously published works and include the addition of hexahydro-1-nitroso-3,5-dinitro-1,3,5-triazine (MNX); hexahydro-1,3-dinitroso-5-nitro-1,3,5-triazine (DNX); hexahydro-1,3,5-trinitroso-1,3,5-triazine (TNX); 2,4-diamino-6-nitrotoluene (2,4-DANT); and 2,6-diamino-4-nitrotoluene (2,6-DANT). One primary analytical method and two secondary (confirmation) methods were developed capable of detecting 29 analytes and two surrogates. Methods for high water concentrations (direct injection), low-level water concentrations (solid phase extraction), soil (solvent extraction), and tissue (solvent extraction) were tested for analyte recovery of the new compounds.