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Title: Improved salting out extraction-preconcentration method for the determination of nitroaromatics and nitramines in water
Authors: U.S. Army Engineer Waterways Experiment Station.
U.S. Army Toxic and Hazardous Materials Agency.
Miyares, Paul H.
Jenkins, Thomas F.
Keywords: Munitions
Munition in water
Water pollution
Groundwater pollution
Salting-out extraction
Nitroaromatic compounds
Publisher: Cold Regions Research and Engineering Laboratory (U.S.)
Engineer Research and Development Center (U.S.)
Series/Report no.: Special report (Cold Regions Research and Engineering Laboratory (U.S.)) ; 91-18.
Description: Special Report
Abstract: An improved salting-out extraction-preconcentration, RP-HPLC-UV protocol for the determination of nitroaromatics and nitramines in water was developed. The method involves saturating a 760-mL water sample with NaCl and extracting with acetonitrile (ACN). Collected extracts are then preconcentrated and solvent exchanged to water via a Kuderna-Danish evaporator. Analysis involves solute focusing by introducing an 1100-mL sample onto a LC-8 (7.5-cm, 3-μm) column eluted with water, MeOH and THF (70.7 : 27.8 : 1.5 [v/v/v]) at 2.0mL/min followed by UV detection at 254nm. A direct injection RP-HPLC-UV water method was developed concurrently, employing the same separation and detection techniques. Both methods are applicable for simultaneous determination of RDX, TNB, DNB, TNT, 2,4-DNT, 2,6-DNT, 2-Am-DNT and 4-Am-DNT, and HMX (salting-out only) with reporting limits ranging from 0.006 to 0.27 μg/L for the salting-out method and 0.12 to 1.07 μg/L for the direct injection method. The salting-out extraction procedure is suitable for determination of HMX, RDX, TNT, 2,4-DNT and 2,6-DNT at concentrations below the health advisory and water quality criteria proposed by the US EPA and Oak Ridge National Laboratory.
Rights: Approved for public release; distribution is unlimited.
Appears in Collections:Special Report

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