7 Aug 2025

Continued Development of Methods for the Determination of Legacy and Insensitive Munitions from Environmental Matrices: Addition of Four Degradation Products and One Internal Standard to Previously Developed 29-Analyte Method

Abstract: To continue improving separation methods of explosive analytes and their degradation products, chromatographic methods from Environmental Protection Agency (EPA) 8330B, Strategic Environmental Research and Development Program (SERDP) 2722, and Environmental Sensors for Explosives were modified to include the separation of four additional analytes and one internal standard so that a total of 36 analytes could be resolved on a single column. Four degradation compounds, 3-amino-1,2,4-triazol-5-one (ATO); 1 methyl-3-nitroguandine (MeNQ); 2 methoxy-5-nitroaniline (MENA); and 4 methoxy-3-nitroaniline (iMENA) were added to the analytical method. The internal standard, 3,5-dinitrotoluene, was also added to the method to extend its application. Additionally, an analytical method on gas chromatography (GC) and gas chromatography–mass spectrometry (GC-MS) were explored for the analytes of interest.

28 Oct 2021

Solid-phase microextraction (SPME) for determination of geosmin and 2-methylisoborneol in volatile emissions from soil disturbance

Abstract: A method is described here for the concentration and determination of geosmin and 2-methylisoborneol (2-MIB) from the gaseous phase, with translation to field collection and quantification from soil disturbances in situ. The method is based on the use of solid-phase microextraction (SPME) fibers for adsorption of volatile chemicals from the vapor phase, followed by desorption into a gas chromatograph-mass spectrometer (GC-MS) for analysis. The use of a SPME fiber allows simple introduction to the GC-MS without further sample preparation. Several fiber sorbent types were studied and the 50/30 μm DVB/CAR/PDMS was the best performer to maximize the detected peak areas of both analytes combined. Factors such as extraction temperature and time along with desorption temperature and time were explored with respect to analyte recovery. An extraction temperature of 30 ◦C for 10 min, with a desorption temperature of 230 ◦C for 4 min was best for the simultaneous analysis of both geosmin and 2-MIB without complete loss of either one. The developed method was used successfully to measure geosmin and 2-MIB emission from just above disturbed and undisturbed soils, indicating that this method detects both compounds readily from atmospheric samples. Both geosmin and 2-MIB were present as background concentrations in the open air, while disturbed soils emitted much higher concentrations of both compounds. Surprisingly, 2-MIB was always detected at higher concentrations than geosmin, indicating that a focus on its detection may be more useful for soil emission monitoring and more sensitive to low levels of soil disturbance.