Document Type

Dissertation

Degree

Doctor of Philosophy (PhD)

Department

Chemistry

First Advisor's Name

Bruce R. McCord

First Advisor's Committee Title

Committee Chair

Second Advisor's Name

John Berry

Second Advisor's Committee Title

Committee Member

Third Advisor's Name

Yong Cai

Third Advisor's Committee Title

Committee Member

Fourth Advisor's Name

Chenzhong Li

Fourth Advisor's Committee Title

Committee Member

Fifth Advisor's Name

Alexander Mebel

Fifth Advisor's Committee Title

Committee Member

Keywords

Chemistry, Explosives, On-Site Detection, Colorimetric, Paper Microfluidics, Electrochemical Detection, Mass Spectrometry

Date of Defense

11-7-2014

Abstract

In recent years, there has been a dramatic increase in the use of improvised explosive devices (IEDs) due to ease of synthesis and improved controls placed on commercial/military explosives. Commonly used materials for IED preparations include fertilizers and industrial chemicals containing oxidizers such as ClO3-, ClO4-, and NO3-, as well as other less stable compounds, such as peroxides. Due to these materials having a wide range of volatility, polarity, and composition, detection can be challenging, increasing the amount of time before any analytical information on the identity of the explosive can be determined. Therefore, this research project developed two analytical methods to aid in the rapid detection of multiple explosive compounds.

The use of microfluidic paper-based analytical devices (µPADs) allows for the development of inexpensive paper devices utilizing colorimetric reactions, which can perform five or more simultaneous analyses in approximately five minutes. Two devices were developed: one for the detection of inorganic explosives including ClO3-, ClO4-, NH4+, NO3-, and NO2-, and the second device detects high/organic explosives including RDX, TNT, urea nitrate, and peroxides. Limits of detection ranged from 0.4 µg – 20 µg of explosive residue with an analysis time of less than five minutes.

Development of a confirmatory method utilizing infusion electrochemical detection-electrospray ionization-time-of-flight mass spectrometry (EC-ESI-TOF MS) and 18-crown-6 ethers to produce guest/host complexes with inorganic ions has also been completed. Utilizing this method the inorganic ions present in many IEDs can be successfully detected as ion pairs, while still allowing for the detection of other high explosives1. Placing an electrochemical detector before the mass spectrometer permits the detection of hydrogen peroxide, an analyte normally difficult to detect through mass spectrometry. Limits of detection ranged from 0.06 ppm - 2 ppm with an analysis time of less than two minutes.

The development of these presumptive and confirmatory analytical methods permits the detection of a wide range of components present in IEDs. These methods decrease the amount of time required to relay information on the type of explosives present by simplifying the analysis process in the field and in a laboratory.

Identifier

FI14110757

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