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Title: Reverse phase HPLC method for analysis of TNT, RDX, HMX and 2,4-DNT in munitions wastewater
Authors: U.S. Army Toxic and Hazardous Materials Agency.
University of New Hampshire. Dept. of Chemistry.
Jenkins, Thomas F.
Bauer, Christopher F.
Leggett, Daniel C.
Grant, Clarence L.
Keywords: DNT
Interlaboratory test
Reverse Phase High Performance Liquid Chromatography
Statistical tests
Test and evaluation
Water testing
Water pollution control
Publisher: Cold Regions Research and Engineering Laboratory (U.S.)
Engineer Research and Development Center (U.S.)
Series/Report no.: CRREL report ; 84-29.
Description: CRREL Report
Abstract: 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 μm polycarbonate membrane and analysis of a 100-μL sub sample 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 and 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 μg/L for HMX, RDX, TNT and 2,4-DNT respectively. Analytical precision was estimated at ± 3.4, 3.3, 4.4 and 4.6 μg/L. 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, wastewater from HMX/RDX manufacture and contaminated groundwater. An interlaboratory test of the method was conducted with nine participating organizations, including laboratories at four Army ammunition plants, the EPA's Environmental Monitoring and Support Laboratory, three Army research organizations and a university. For the four analytes collectively, the analytical accuracy was within 5%, the intralaboratory precision (repeatability) was 5 to 9% based on the average of duplicate injections, and the interlaboratory precision (reproducibility) was 7 to 10%. This evaluation excluded about 10% of the data, which were identified as outliers.
Appears in Collections:CRREL Report

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