Issue 8, 2010

Determination of peroxide-based explosives with copper(ii)–neocuproine assay combined with a molecular spectroscopic sensor

Abstract

The two members of peroxide-based explosives, triacetone triperoxide (TATP) and hexamethylene triperoxide diamine (HMTD), can be manufactured from readily accessible reagents, and are difficult to detect by conventional analytical methods. TATP and HMTD were securely synthesized, taken up with acetone, hydrolyzed with 4 M HCl to hydrogen peroxide, the acidic solution containing H2O2 was neutralized, and assayed by the copper(II)neocuproine spectrophotometric method. The chromophore of the reaction was the Cu(I)neocuproine chelate responsible for light absorption at 454 nm. The molar absorptivity (ε) of the method for TATP and HMTD was 3.45 × 104 and 4.68 × 104 L mol−1 cm−1, respectively. The TATP recovery from a synthetically contaminated loamy clay soil was 91–99%. The colorimetric method was also applied to a Cu(II)neocuproine-impregnated polymeric Nafion membrane sensor developed for the first time in this work for peroxide explosive assay. The absorbance–concentration response was perfectly linear, and the limit of detection (LOD) of the procedure for both TATP and HMTD was approximately 0.2 mg L−1. Neither common soil ions (Ca2+, K+, Cl, SO42−, Mg2+ and NO3) at 100-fold amounts nor military-purpose nitro-explosives of TNT, RDX, and PETN at 10-fold amounts interfered with the proposed assay. Active oxygen constituents of laundry detergents (perborates and percarbonates), which normally interfered with the assay, could easily be separated from the analytes by solubility differences. The method was statistically validated against standard reference methods of TiOSO4 colorimetry and GC-MS.

Graphical abstract: Determination of peroxide-based explosives with copper(ii)–neocuproine assay combined with a molecular spectroscopic sensor

Article information

Article type
Paper
Submitted
07 Dec 2009
Accepted
13 May 2010
First published
07 Jun 2010

Analyst, 2010,135, 2085-2091

Determination of peroxide-based explosives with copper(II)neocuproine assay combined with a molecular spectroscopic sensor

Ş. Eren, A. Üzer, Z. Can, T. Kapudan, E. Erçağ and R. Apak, Analyst, 2010, 135, 2085 DOI: 10.1039/B925653A

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