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Full-Text Articles in Analytical Chemistry

Structure Elucidation Of A Pyrrolobenzodiazepine Alkaloid And A Biologically Active Polyketide Produced By Rhodococcus Sp. Mtm3w5.2 Via Two-Dimensional Nmr Spectroscopy, Garrett Johnson Dec 2019

Structure Elucidation Of A Pyrrolobenzodiazepine Alkaloid And A Biologically Active Polyketide Produced By Rhodococcus Sp. Mtm3w5.2 Via Two-Dimensional Nmr Spectroscopy, Garrett Johnson

Electronic Theses and Dissertations

As the battle against ever-increasing drug resistence bacteria rages on, novel and sometimes more complex natural products can be used to combat this. In this study, two-dimensional NMR techniques were utilized to collect a complete spectral data set for two natural products. The first structure, a synthesized Pyrrolobenzodiazepine alkaloid natural product was confirmed through these methods. The second, a strain of Rhodococcus, MTM3W5.2, produces a novel antibacterial molecule in broth cultures and the active compound was fractionated using a Sephedex LH-20 column. Chromatographic purification yielded a pure sample at 58.90 minutes, RT.58. HRMS data deduced an exact mass of …


Electrodeposition Of Hydrogen Molybdenum Bronze Films And Electrochemical Reduction Of Carbon Dioxide At Low Over Potentials, Sami Alharbi Aug 2019

Electrodeposition Of Hydrogen Molybdenum Bronze Films And Electrochemical Reduction Of Carbon Dioxide At Low Over Potentials, Sami Alharbi

Electronic Theses and Dissertations

Hydrogen molybdenum oxide, known has molybdenum bronze, is a material of interest due to catalyzing electron transfer reactions. Specifically, molybdenum bronze is an electrocatalyst toward carbon dioxide reduction. Electrochemical deposition from a peroxymolybdic acid solution is a method for preparing molybdenum bronze films. This work demonstrates reproducible electrodeposition on indium tin oxide substrates and conductive carbon paper. Film thickness depends on concentration, time and pH. After characterization by film thickness, resistance, XRD and XPS, the as deposited films served as the working electrode for electrochemical reduction of carbon dioxide in 0.1 M NaHCO3. Ion chromatography determined formate resulting …


Modification Of Chemical Vapor-Deposited Carbon Electrodes With Electrocatalytic Metal Nanoparticles Through A Soft Nitriding Technique, Enoch Amoah Aug 2019

Modification Of Chemical Vapor-Deposited Carbon Electrodes With Electrocatalytic Metal Nanoparticles Through A Soft Nitriding Technique, Enoch Amoah

Electronic Theses and Dissertations

Metal nanoparticles have been widely used for many catalytic and electrocatalytic applications due to their larger surface area-to-volume ratios and higher densities of active sites compared to bulk materials. This has resulted in much interest in understanding the electrocatalytic behavior of metal nanoparticles with respect to their structure. However, most research on this topic has employed collections of nanoparticles. Due to difficulties in controlling and characterizing particle loading and interparticle distance in nanoparticle ensembles, single nanoparticles studies have recently become a topic of great interest. In this study, a soft nitriding technique was applied to chemical vapor-deposited carbon ultramicroelectrodes (UMEs) …


Peroxide Sensing Using Nitrogen-Doped And Platinum Nanoparticle-Modified Screen-Printed Carbon Electrodes, Chidiebere Ogbu Aug 2019

Peroxide Sensing Using Nitrogen-Doped And Platinum Nanoparticle-Modified Screen-Printed Carbon Electrodes, Chidiebere Ogbu

Electronic Theses and Dissertations

Nitrogen-doped carbon materials have garnered much interest due to their abilities to behave as electrocatalysts for reactions important in energy production (oxygen reduction) and biosensing (hydrogen peroxide reduction). Here, we demonstrate fabrication methods and determine electrocatalytic properties of nitrogen-doped screen-printed carbon (N-SPCE) electrodes. Nitrogen doping of graphite was achieved through a simple soft-nitriding technique which was then used in lab-formulated screen-printing inks to prepare N-SPCEs. N-SPCEs displayed good electrocatalytic activity, reproducibility and long term stability towards the electrochemical reduction of hydrogen peroxide. N-SPCEs exhibited a wide linear range (20 µM to 5.3 mM), reasonable limit of detection of 2.5 µM, …


Immobilization Of Electrocatalytically Active Gold Nanoparticles On Nitrogen-Doped Carbon Fiber Electrodes, Daniel Mawudoku Aug 2019

Immobilization Of Electrocatalytically Active Gold Nanoparticles On Nitrogen-Doped Carbon Fiber Electrodes, Daniel Mawudoku

Electronic Theses and Dissertations

Studies of single, isolated nanoparticles provide better understanding of the structure-function relationship of nanoparticles since they avoid complications like interparticle distance and nanoparticle loading that are typically associated with collections of nanoparticles distributed on electrode supports. However, interpretation of results obtained from single nanoparticle immobilization studies can be difficult to interpret since the underlying nanoelectrode platform can contribute to the measured current, or the immobilization technique can adversely affect electron transfer. Here, we immobilized ligand-free gold nanoparticles on relatively electrocatalytically inert nitrogen-doped carbon ultramicroelectrodes that were prepared via a soft nitriding method. Sizes of the particles were estimated by a …


Gas Chromatography Analysis Of Co2 Reduction Photocatalysis With Zinc Dipyrrin Complexes, Alex Day May 2019

Gas Chromatography Analysis Of Co2 Reduction Photocatalysis With Zinc Dipyrrin Complexes, Alex Day

Undergraduate Honors Theses

Bis(1,3,7,9-tetramethyl-5-mesityldipyrrinato)zinc(II) (ZnDPY) was synthesized in the lab by the McCusker group and a procedure was created to analyze its ability as a photosensitizer, a molecule that provides the energy for the reaction to occur by capturing light energy and turning it into a form that can be used by the photocatalyst. While more work is needed, preliminary steps have been made to create a process that can analyze the amount of carbon monoxide produced by a photocatalytic CO2 reduction reaction with ZnDPY as the photosensitizer. Progress has been made via the setup of a reaction apparatus, targeted gas chromatography …


Development Of Granulated Adsorbent For Clean-Up Of Water Contaminated By Cesium, Esther Alorkpa May 2019

Development Of Granulated Adsorbent For Clean-Up Of Water Contaminated By Cesium, Esther Alorkpa

Electronic Theses and Dissertations

A study was conducted on sol-gel synthesis of an adsorbent (phosphotungstic acid embedded in silica gel, H-PTA/SiO­2) of radioactive cesium. A novelty of this work is covalent bonding of PTA to the surface of solid support that prevents leaching from the surface of the material. The sample was granulated with a binder, aluminium oxide (γ-Al2O3). Solid-state NMR and FT-IR spectroscopy were used to confirm the presence of Keggin units of PTA in the bound materials. Thermal analysis of H-PTA/SiO­2 - γ-Al2O3 (50 %) showed that the water content in the …