Dr. Ronita L. Marple Profile

Dr. Ronita L. Marple

Graduate Student at Univ of Maryland/Baltimore Co

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Proceedings Article | 7 December 2004 Paper

Determination of organic nitro compounds using HPLC-UV-PAED

Ronita Marple, William LaCourse

Proceedings Volume 5588, (2004) https://doi.org/10.1117/12.571355

KEYWORDS: Ultraviolet radiation, Ultraviolet detectors, Electrodes, Explosives, Sensors, Matrices, Polishing, Photolysis, Lamps, Mode conditioning cables

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High-performance liquid chromatography with ultra violet and photo-assisted electrochemical detection (HPLC-UV-PAED) has been applied to the sensitive and selective determination of organic nitro compounds. The system was first developed for the determination of nitro explosives, and PAED has shown superior sensitivity over UV detection for these compounds (i.e., <1 part-per-trillion for HMX). The system also shows enhanced selectivity over the traditional UV method in that two detectors can be used for improved analyte identification. Also, having two detectors permits chemometric resolution of overlapping peaks, and this is not addressed in the UV method. Because this method is applicable to a wide range of nitro explosives, it was predicted that PAED would show the same sensitivity and selectivity toward other types of nitro compounds. Since its development, the system's use has been expanded to include the determination of nitro-containing pharmaceuticals and glycosylated nitro compounds in biological matrices. Model compounds were chosen, specifically nitroglycerin and related compounds and nitrophenyl-glucoside, to represent these classes. PAED showed superior detection limits over low wavelength UV detection for nitroglycerin (PAED = 0.3ppb, UV at 220nm = 48ppb), demonstrating PAED’s applicability to determining nitro-pharmaceuticals. Conversely, UV detection at 220nm proved to be more sensitive than PAED for nitrophenyl-glucoside (UV at 220 = 0.6ppb, PAED = 3.6ppb). However, when nitrophenyl-glucoside was spiked into urine, PAED determination resulted in 99+0.3% recovery, while UV at 220nm resulted in 116+0.2% recovery, suggesting that UV determination may suffer from matrix interference.

Proceedings Article | 4 March 2004 Paper

On-site comprehensive analysis of explosives using HPLC-UV-PAED

Ronita Marple, William LaCourse

Proceedings Volume 5270, (2004) https://doi.org/10.1117/12.516186

KEYWORDS: Explosives, Soil contamination, Soil science, Ultraviolet radiation, Sensors, Statistical analysis, Sodium, Solids, Environmental sensing, Ultraviolet detectors

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High-performance liquid chromatography with ultra violet and photo-assisted electrochemical detection (HPLC-UV-PAED) has been developed for the sensitive and selective detection of explosives in ground water and soil extracts. Fractionation and preconcentration of explosives is accomplished with on-line solid phase extraction (SPE), which minimizes sample pretreatment and enables faster and more accurate on-site assessment of a contaminated site. Detection limits are equivalent or superior (i.e., <1 part-per-trillion for HMX) to those achieved using the Environmental Protection Agency (EPA) Method 8330. This approach is more broadly applicable, as it is capable of determining a wider range of organic nitro compounds. Soil samples are extracted using pressurized fluid extraction (PFE), and this technique is automatable, field-compatible, and environmentally friendly, adding to the overall efficiency of the methodology.

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