Validation of Sample Extraction and Analysis Techniques for Simultaneous Determination of Legacy and IM Constituents

Dr. Anthony Bednar | US Army Engineer Research and Development Center

ER19-5078

Objective

This project will demonstrate and validate an extraction and analytical method for the simultaneous analysis of Insensitive Munitions (IM) and legacy energetic compounds, developed under the Strategic Environmental Research and Development Program (SERDP) project ER-2722, and transition this method to the USEPA for standardization across Department of Defense (DoD) contract and research laboratories as an option in USEPA Method 8330. As the use of IM increases, their analysis in environmental matrices becomes more important, and because IM are manufactured at the same facilities or used on ranges or sites where legacy materials remain, there is a need to simultaneously quantify IM and legacy explosives.

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Technology Description

A high performance liquid chromatography (HPLC) method, with requisite extraction procedures, has been developed through in-house ERDC and SERDP funded research, based on USEPA Method 8330, the current standard method for determination of legacy energetic compounds. The method, as optimized under SERDP ER-2722, allows direct simultaneous analysis of IM and Legacy compounds in water at levels above ~20 μg/L, analysis in waters below 20 μg/L (e.g. ~0.2 μg/L with a 100x SPE concentration factor) after solid phase extraction (SPE), and in soils, sediments, and tissues after solvent extraction. Specifically:

  • Task 1 will result in documented acceptance of the method by USEPA OSW and the organics working group as a practical modification to Method 8330.
  • Task 2 will result in inter-laboratory method transfer and refinement, with acceptable recovery limit range targets as currently defined in the DoD Quality Systems Manual (QSM) Version 5.1 of 57-135% (waters) and 64-135% (solids), duplicate relative standard deviations < 20%, and other laboratory QC results within QSM limits.
  • Task 3 will result in acceptance of the combined IM and legacy extraction and analysis method through technology transfer in the form of an addendum to USEPA Method 8330 submitted to USEPA, with inter-laboratory performance data, as well as dissemination through presentations at the DoD Environmental Monitoring and Data Quality workgroup (EMDQ) and an ESTCP webinar for user awareness and familiarization.

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Benefits

There is currently no standard method for determination of IM energetic compounds in environmental matrices, resulting in the use of multiple, non-standard methods, leading to potentially compromised data and higher resource and labor costs. By providing a standard method for simultaneous legacy and IM compound determinations results in cost savings and known data quality. Obtaining regulatory approval of the combined legacy and IM extraction and analytical method will provide laboratories and the user community options for analyses. The dual procedure availability will minimize costs by allowing laboratories to use just one analytical technique, depending on their current need. In addition, widespread utilization of the method will allow environmental issues associated with the IM lifecycle to be identified early with a standardized and accepted technique. Finally, the technique will be transferred to USEPA Method 8330 as an option, rather than a requirement, such that when only legacy compound analysis is required, the current standard method will still be available.

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Points of Contact

Principal Investigator

Dr. Anthony Bednar

U.S. Army Engineer Research and Development Center (ERDC)

Phone: 601-634-3652

Fax: 601-634-2747

Program Manager

Environmental Restoration

SERDP and ESTCP

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