Determination of nitroaromatic and nitramine type energetic materials in synthetic and real mixtures by cyclic voltammetry

Nitro-explosives contain reducible aromatic -NO2 groups or cyclic >N-NO2 bonds that may undergo reductive cleavage. This work reports the development of a cyclic voltammetric (CV) assay for nitro-aromatics (trinitrotoluene (TNT), dinitrotoluene (DNT)) and nitramines (1,3,5-trinitro-1,3,5-triazacyclohexane (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX)) using a glassy carbon electrode. This determination was first used for these energetic materials by resolving current responses of reduction potentials primarily due to one constituent but partly contributed by other constituents. Calibration curves of current intensity versus concentration were linear in the range of 30-120 mg L-1 for RDX with a limit of detection (LOD) of 10.2 mg L-1, 40-120 mg L-1 for HMX (LOD=11.7 mg L-1), 40-120 mg L-1 for TNT (LOD=11.2 mg L-1), and 40-140 mg L-1 for DNT (LOD=10.8 mg L-1). Results showed that the CV method could provide a sensitive approach for the simultaneous determination of RDX and TNT in synthetic and real mixtures. Deconvolution of current contributions of mixtures at peak potentials of constituents was performed by multiple linear regression. The proposed method was successfully applied to the analysis of military explosives comp A5 and octol, and method validation was performed both against HPLC on a comp B (TNT+RDX) sample and against GC-MS on real post-blast residual samples containing both explosives. (C) 2013 Elsevier B.V. All rights reserved

The effect of reduction methods and stabilizer (PVP) on the properties of polyacrylonitrile (PAN) composite nanofibers in the presence of nanosilver

There are many studies which use different types of reduction methods that affect the final properties of composite material containing silver nitrate (AgNO3). The use of poly(N-vinylpyrrolidone) (PVP) in the composite also affects the final properties of composite material. However, as seen from the literature, it is difficult to find any studies focusing on polymer composite nanofibers reduced using different reduction methods and studies with different PVP loadings which are compared to each other, although it is very important to determine the most suitable reduction method and PVP loading for final composite properties. Thus, in this work, the effect of different reduction methods on polyacrylonitrile (PAN) composite nanofibers incorporating AgNO3 and the comparison of different amounts of stabilizer (PVP) are studied in detail to determine the most suitable reduction method and the effect of PVP loading on the structure and the properties of the final product. PAN composite nanofibers having different amounts of PVP are reduced by four different methods namely arc-sol method, hydrazine method, arc-web method, and reflux method and characterized by electrical conductivity, mechanical testing, and thermal and SEM analyses. It has been observed that the hydrazine method provides higher breaking strength, electrical conductivity, enthalpy, smallest diameter, and lower cyclization temperature (T (c)) than other reduction methods. Presence of PVP results in an increase of breaking strength and cyclization temperature, a decrease of enthalpy and the electrical conductivity. While highest breaking strength was obtained by hydrazine reduction with highest PVP loading, highest electrical conductivity was obtained by hydrazine reduction without PVP. As a direct result of the incorporation of AgNO3 with or without PVP, insulator pure PAN (10(-12) S/cm) becomes semi-conductive material (10(-7) S/cm), which can be used as an antistatic material