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1.
Anal Chim Acta ; 661(1): 117-21, 2010 Feb 19.
Article in English | MEDLINE | ID: mdl-20113724

ABSTRACT

This article reports on an integrated explosive-preconcentration/electrochemical detection system for 2,4,6-trinitrotoluene (TNT) vapor. The challenges involved in such system integration are discussed. A hydrogel-coated screen-printed electrode is used for the detection of the thermally desorbed TNT from a preconcentration device using rapid square wave voltammetry. Optimization of the preconcentration system for desorption of TNT and subsequent electrochemical detection was conducted yielding a desorption temperature of 120 degrees C under a flow rate of 500 mL min(-1). Such conditions resulted in a characteristic electrochemical signal for TNT representing the multi-step reduction process. Quantitative measurements produced a linear signal dependence on TNT quantity exposed to the preconcentrator from 0.25 to 10 microg. Finally, the integrated device was successfully demonstrated using a sample of solid TNT located upstream of the preconcentrator.


Subject(s)
Electrochemistry/instrumentation , Explosive Agents/chemistry , Trinitrotoluene/chemistry , Electrochemistry/methods , Explosive Agents/analysis , Trinitrotoluene/analysis , Volatilization
2.
Nano Lett ; 10(2): 380-4, 2010 Feb 10.
Article in English | MEDLINE | ID: mdl-20041699

ABSTRACT

Real-time detection of trace chemicals, such as explosives, in a complex environment containing various interferents has been a difficult challenge. We describe here a hybrid nanosensor based on the electrochemical reduction of TNT and the interaction of the reduction products with conducting polymer nanojunctions in an ionic liquid. The sensor simultaneously measures the electrochemical current from the reduction of TNT and the conductance change of the polymer nanojunction caused from the reduction product. The hybrid detection mechanism, together with the unique selective preconcentration capability of the ionic liquid, provides a selective, fast, and sensitive detection of TNT. The sensor, in its current form, is capable of detecting parts-per-trillion level TNT in the presence of various interferents within a few minutes.


Subject(s)
Conductometry/instrumentation , Electrochemistry/methods , Environmental Monitoring/instrumentation , Environmental Monitoring/methods , Nanotechnology/methods , Polymers/chemistry , Chromatography, High Pressure Liquid , Electrolytes , Explosive Agents , Ions , Spectroscopy, Fourier Transform Infrared
3.
Analyst ; 134(3): 528-32, 2009 Mar.
Article in English | MEDLINE | ID: mdl-19238290

ABSTRACT

This article describes an effective microchip protocol based on electrophoretic-separation and electrochemical detection for highly sensitive and rapid measurements of nitrate ester explosives, including ethylene glycol dinitrate (EGDN), pentaerythritol tetranitrate (PETN), propylene glycol dinitrate (PGDN) and glyceryl trinitrate (nitroglycerin, NG). Factors influencing the separation and detection processes were examined and optimized. Under the optimal separation conditions obtained using a 15 mM borate buffer (pH 9.2) containing 20 mM SDS, and applying a separation voltage of 1500 V, the four nitrate ester explosives were separated within less than 3 min. The glassy-carbon amperometric detector (operated at -0.9 V vs. Ag/AgCl) offers convenient cathodic detection down to the picogram level, with detection limits of 0.5 ppm and 0.3 ppm for PGDN and for NG, respectively, along with good repeatability (RSD of 1.8-2.3%; n = 6) and linearity (over the 10-60 ppm range). Such effective microchip operation offers great promise for field screening of nitrate ester explosives and for supporting various counter-terrorism surveillance activities.


Subject(s)
Explosive Agents/analysis , Nitrates/analysis , Electrochemical Techniques/methods , Electrophoresis, Microchip/instrumentation , Electrophoresis, Microchip/methods , Esters/analysis , Forensic Sciences/instrumentation , Forensic Sciences/methods , Sensitivity and Specificity
4.
Analyst ; 133(5): 585-7, 2008 May.
Article in English | MEDLINE | ID: mdl-18427677

ABSTRACT

A highly selective and rapid electrochemical assay of the improvised explosive urea nitrate (UN) is reported. The method involves a short ( approximately 10 s) acid-catalyzed reaction of UN with 4-nitrotoluene (NT) followed by a rapid ( approximately 2 s) square-wave voltammetric (SWV) detection of the 2,4-dinitrotoluene (DNT) product. The new protocol offers great promise for a reliable field detection of UN, with significant advantages of speed, sensitivity, portability, simplicity, and cost.


Subject(s)
Explosive Agents/analysis , Nitrates/analysis , Security Measures , Urea/analogs & derivatives , Dinitrobenzenes/analysis , Electrochemistry/methods , Electronic Data Processing , Explosive Agents/chemistry , Nitrates/chemistry , Toluene/analogs & derivatives , Toluene/chemistry , Urea/analysis , Urea/chemistry
5.
Analyst ; 132(6): 560-5, 2007 Jun.
Article in English | MEDLINE | ID: mdl-17525813

ABSTRACT

A fast, simple and sensitive electrochemical method for sensing peroxide-based explosives based on their acid treatment is reported. The method relies on the high electrocatalytic activity of Prussian-blue (PB)-modified electrodes towards the acid-generated hydrogen peroxide in the harsh acidic medium (down to pH 0.3) used for releasing hydrogen peroxide. Such effective operation of PB electrochemical sensors in strongly acidic media eliminates the need for an additional neutralization step required in analogous peroxidase-based assays (due to acid-induced enzyme deactivation processes). Factors affecting the efficiency of the acid pre-treatment of triacetone triperoxide (TATP) have been examined and optimized to allow its sensitive measurement down to the 50 ng level within 60 s. Chronoamperometric detection of microgram amounts of solid TATP, following a one-minute acid mixing and placing a 20 microL droplet onto a disposable PB-modified screen-printed electrode is illustrated. Similar results were obtained for the peroxide explosive hexamethylene triperoxide diamine (HMTD). By greatly simplifying the analytical procedure, such an acid-operated "artificial peroxidase" electrocatalytic transducer holds great promise for designing "one-step", user-friendly, miniaturized, cost-effective devices for field screening of peroxide explosives.


Subject(s)
Explosive Agents/analysis , Heterocyclic Compounds, 1-Ring/analysis , Peroxides/analysis , Electrochemistry/instrumentation , Electrochemistry/methods , Electrodes , Ferrocyanides , Hydrogen Peroxide/analysis , Hydrogen-Ion Concentration , Indicators and Reagents
6.
Analyst ; 131(12): 1279-81, 2006 Dec.
Article in English | MEDLINE | ID: mdl-17124534

ABSTRACT

A highly sensitive electrochemical assay of the peroxide-based explosives triacetone triperoxide (TATP) and hexamethylene triperoxide diamine (HMTD) at a Prussian-blue (PB) modified electrode is reported. The method involves photochemical degradation of the peroxide explosives and a low potential (0.0 V) electrocatalytic amperometric sensing of the generated hydrogen peroxide at the PB transducer and offers nanomolar detection limits following a short (15 s) irradiation times. The electrochemical sensing protocol should facilitate rapid field screening of peroxide explosives.


Subject(s)
Explosive Agents/analysis , Hydrogen Peroxide/analysis , Bridged Bicyclo Compounds, Heterocyclic/analysis , Carbon , Electrochemistry , Electrodes , Ferrocyanides , Heterocyclic Compounds, 1-Ring/analysis , Peroxides/analysis , Platinum
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