Nitramine residues

Jenkins TF, Walsh ME, Schumacher PW, et al. 1989. Liquid chromatographic method for determination of extractable nitroaromatic and nitramine residues in soil. J Assoc Off Anal Chem 72 890- 899. 

Seven priority pollutant nitroaromatic (nitrobenzene and nitro-, nitroamino-, and dinitrotoluene) and nitramine residues (i.e., HMX, RDX, TNBA, TNB, DNB, Tetryl, TNT) were extracted from soil and separated on a C j column (A = 254 nm) using a 50/50 methanol/water mobile phase [180]. Retention times ranged from 2 to 15 min. Detection limits varied from 1 to 30ng/g (analyte dependent). The linear working range was reported as 10-10,000 pg/g. This study is extremely important in that it also describes in detail the effects of numerous operating parameters (e.g., sample and standard stability, matrix effects). 

Dark Decay of UDMH in the Presence of NO, When 1.3 ppm of UDMH in air was reacted in the dark with an approximately equal amount of NO, 0.25 ppm of UDMH was consumed and formation of -0.16 ppm HONO and -0.07 ppm N2O was observed after -3 hours. Throughout the reaction, a broad infrared absorption at -988 cm" corresponding to an unidentified product(s), progressively grew in intensity. The residual infrared spectrum of the unknown product(s) is shown in Figure 2a. It is possible that a very small amount (50.03 ppm) of N-nitrosodimethylamine could also have been formed but the interference by the absorptions of the unknown product(s) made nitrosamine (as well as nitramine) detection difficult. No significant increase in NH3 levels was observed, in contrast to the UDMH dark decay in the absence of NO. Approximately 70% of the UDMH remained at the end of the 3-hour reaction period this corresponds to a half-life of -9 hours which is essentially the same decay rate as that observed in the absence of NO. 

Grant et al. [30] found that nitramine and nitroaromatic explosive residues in real field soil samples were stable under refrigeration, but nitroaromatics used to fortify samples degraded rapidly, even when samples were refrigerated. Therefore, fortified soils can lead to significant errors. 

Bratin, K., P. T. Kissinger, R. Briner, and C. Bruntlett. Determination of nitro aromatic, nitramine, and nitrate ester explosive compounds in explosives mixtures and gunshot residue by liquid-chromatography and reductive electrochemical detection. Anal. Chim. Acta 130, 295-311 (1981). 

K. Bratin, P. T. Kissinger, R. C. Briner, and C. S. Bruntlett, Determination of Nitro Aromatic, Nitramine and Nitrate Ester Explosive Compounds in Explosive Mixtures and Gunshot Residue by Liquid Chromatography and Reductive Electrochemical Detection, Analytica Chimica Acta 130, no. 2 (1981) 295. 

MC found primarily at impact areas and tiring lines of U.S. military testing and training ranges often consist of mixtures of residues from several MC. These may include the nitroaromatic explosive compounds 2,4,6-trinitrotoluene (TNT), 2,4- and 2,6-dinitro-toluene (DNT), and trinitrophenylmethylnitramine (tetryl) nitrate esters such as nitrocellulose (NC), pentaerythritol tetranitrate (PETN), and nitroglycerin (NG) and the nitramine compounds, hexahydro-l,3,5-trinitro-l,3,5-triazine (RDX) and octahydro-l,3,5,7-tetranitro-l,3,5,7-tetrazocine (HMX). Most of these MC have been in use for decades, either as primary or secondary explosives or in propellant compositions. 

EC reduction has been used extensively in the detection of residues of nitro-aromatic, nitramine, and nitrate explosives at pendent Hg, Au amalgam or glassy carbon electrodes - the forensic evaluation of this subject has been reviewed. " The methodology described may be applicable to drugs and other compounds containing these functional groups. 

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