Reverse Phase HPLC Method for Analysis of TNT, RDX, HMX and 2,4-DNT in Munitions Wastewater,
COLD REGIONS RESEARCH AND ENGINEERING LAB HANOVER NH
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An analytical method was developed to determine the concentrations of HMX, RDX, TNT and 2, 4-DNT in munitions wastewater. The method involves dilution of an aqueous sample with an equal volume of methanol-acetonitrile solvent mixture, filtration through a 0.4 micrometer polycarbonate membrane and analysis of a 100 microliter subsample by Reverse-phase, high-performance liquid chromatography using an LC-8 column. Retention times of these four analytes, their degradation products, and impurities expected in wastewater matrices were determined for two eluent compositions. An eluent of 50 water, 38 methanol and 12 acetonitrile successfully separated HMX, RDX, TNT from each other and the potential interferents. The method provided linear calibration curves over a wide range of concentrations. Detection limits were conservatively estimated to be 26, 22,14 and 10 microgramsL for HMX, RDX, TNT 2,4-DNT respectively. Analytical precision was estimated at or - 3.4, 3.3, 4.4 and 4.6 microliterL. A ruggedness test involving the major manipulative steps in the procedure indicated that use of glass sampling containers, the portion of filtrate chosen for analysis and a carefully measured sample-to-organic-solvent ratio was necessary to obtain consistent analytical results. The method was tested with munition wastewater from several Army ammunition plants and found to perform adequately for load and pack wastewaters for load and pack wastewaters, wastewater from HMXRDX manufacture and contaminated groundwater.
- Physical Chemistry
- Ammunition and Explosives
- Water Pollution and Control