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Lipidomic Analysis of Single Cells and Organelles Using Nanomanipulation Coupled to Mass Spectrometry

Description: The capability to characterize disease states by way of determining novel biomarkers has led to a high demand of single cell and organelle analytical methodologies due to the unexpected heterogeneity present in cells of the same type. Lipids are of particular interest in the search for biomarkers due to their active roles in cellular metabolism and energy storage. Analyzing localized lipid chemistry from individual cells and organelles is challenging however, due to low analyte volume, limited discriminate instrumentation, and common requirements of separation procedures and expenditure of cell sample. Using nanomanipulation in combination with mass spectrometry, individual cells and organelles can be extracted from tissues and cultures in vitro to determine if heterogeneity at the cellular level is present. The discriminate extraction of a single cell or organelle allows the remainder of cell culture or tissue to remain intact, while the high sensitivity and chemical specificity of mass spectrometry provides structural information for limited volumes without the need for chromatographic separation. Mass analysis of lipids extracted from individual cells can be carried out in multiple mass spectrometry platforms through direct-inject mass spectrometry using nanoelectrospray-ionization and through matrix-assisted laser/desorption ionization.
Date: May 2016
Creator: Bowman, Amanda
Partner: UNT Libraries

Electrochemical Synthesis and Applications of Layered Double Hydroxides and Derivatives

Description: Layered double hydroxides (LDH) are a class of anionic clay with alternating layers of positive and negative charge. A metal hydroxide layer with divalent and trivalent metals with a positive charge is complemented by an interlayer region containing anions and water with a negative charge. The anions can be exchanged under favorable conditions. Hydrotalcite (Mg6Al2(OH)16[CO3]·4H2O) and other variations are naturally occurring minerals. Synthetic LDH can be prepared as a powder or film by numerous methods. Synthetic LDH is used in electrode materials, adsorbents, nuclear waste treatment, drug delivery systems, water treatment, corrosion protection coatings, and catalysis. In this dissertation Zn-Al-NO3 derivatives of zaccagnaite (Zn4Al2(OH)12[CO3]·3H2O) are electrochemically synthesized as films and applied to sensing and corrosion resistance applications. First, Zn-Al-NO3 LDH was potentiostatically electrosynthesized on glassy carbon substrates and applied to the electrochemical detection of gallic acid and caffeic acid in aqueous solutions. The modified electrode was then applied to the detection of gallic acid in green tea samples. The focus of the work shifts to corrosion protection of stainless steel. Modified zaccagnaite films were electrodeposited onto stainless steel in multiples layers to reduce defects caused by drying of the films. The films were deposited using a step potential method. The corrosion resistance of the films in a marine environment was investigated while immersed in 3.5 wt.% NaCl environments. Next modified zaccagnaite films were potentiostatically electrodeposited onto stainless steel followed by a hydrophobization reaction with palmitic acid in order to prepare superhydrophobic (>150° contact angle) surfaces. Each parameter of the film synthesis was optimized to produce a surface with the highest possible contact angle. The fifth chapter examines the corrosion resistance of the optimized superhydrophobic film and a hydrophobic film. The hydrophobic film is prepared using the same procedure as the superhydrophobic film except for a difference in electrodeposition potential. The ...
Date: August 2015
Creator: Kahl, Michael S.
Partner: UNT Libraries

Interfacial Electrochemistry of Cu/Al Alloys for IC Packaging and Chemical Bonding Characterization of Boron Doped Hydrogenated Amorphous Silicon Films for Infrared Cameras

Description: We focused on a non-cooling room temperature microbolometer infrared imaging array device which includes a sensing layer of p-type a-Si:H component layers doped with boron. Boron incorporation and bonding configuration were investigated for a-Si:H films grown by plasma enhanced chemical deposition (PECVD) at varying substrate temperatures, hydrogen dilution of the silane precursor, and dopant to silane ratio using multiple internal reflection infrared spectroscopy (MIR-IR). This study was then confirmed from collaborators via Raman spectroscopy. MIR-IR analyses reveal an interesting counter-balance relationship between boron-doping and hydrogen-dilution growth parameters in PECVD-grown a-Si:H. Specifically, an increase in the hydrogen dilution ratio (H2/SiH4) or substrate temperature was found to increase organization of the silicon lattice in the amorphous films. It resulted in the decrease of the most stable SiH bonding configuration and thus decrease the organization of the film. The new chemical bonding information of a-Si:H thin film was correlated with the various boron doping mechanisms proposed by theoretical calculations. The study revealed the corrosion morphology progression on aluminum alloy (Al, 0.5% Cu) under acidic chloride solution. This is due to defects and a higher copper content at the grain boundary. Direct galvanic current measurement, linear sweep voltammetry (LSV), and Tafel plots are used to measure corrosion current and potential. Hydrogen gas evolution was also observed (for the first time) in Cu/Al bimetallic interface in areas of active corrosion. Mechanistic insight that leads to effective prevention of aluminum bond pad corrosion is explored and discussed. (Chapter 4) Aluminum bond pad corrosion activity and mechanistic insight at a Cu/Al bimetallic interface typically used in microelectronic packages for automotive applications were investigated by means of optical and scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and electrochemistry. Screening of corrosion variables (temperature, moisture, chloride ion concentration, pH) have been investigated to find their effect on ...
Date: May 2016
Creator: Ross, Nick Mark
Partner: UNT Libraries

Investigation of Novel Electrochemical Synthesis of Bioapatites and Use in Elemental Bone Analysis

Description: In this research, electrochemical methods are used to synthesize the inorganic fraction of bone, hydroxyapatite, for application in biological implants and as a calibration material for elemental analysis in human bone. Optimal conditions of electrochemically deposited uniform apatite coatings on stainless steel were investigated. Apatite is a ceramic with many different phases and compositions that have beneficial characteristics for biomedical applications. Of those phases hydroxyapatite (HA) is the most biocompatible and is the primary constituent of the inorganic material in bones. HA coatings on metals and metal alloys have the ability to bridge the growth between human tissues and implant interface, where the metal provides the strength and HA provides the needed bioactivity. The calcium apatites were electrochemically deposited using a modified simulated body fluid adjusted to pH 4-10, for 1-3 hours at varying temperature of 25-65°C while maintaining cathodic potentials of -1.0 to -1.5V. It was observed that the composition and morphology of HA coatings change during deposition by the concentration of counter ions in solution, pH, temperature, applied potential, and post-sintering. The coatings were characterized by powder x-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy. The precipitated powders from the experiment were also characterized, with results showing similarities to biological apatite. There is a need for quantitative elemental analysis of calcified biological matrices such as bone and teeth; however there are no suitable calibration materials commercially available for quantitative analysis. Matrix-matched standards are electrochemically synthesized for LA-ICP-MS analysis of human bone. The synthetic bioapatite is produced via a hydrothermal electrochemical process using a simulated body fluid solution to form hydroxyapatite. Additional bioapatite standards are synthesized containing trace amounts of metals. The x-ray diffraction of the synthesized standards shows an increase in cell volume for the crystal structure from 0.534 to 0.542 nm3 with the substitution of ...
Date: December 2012
Creator: DeLeon, Vallerie H.
Partner: UNT Libraries

Electrodeposition of Nickel and Nickel Alloy Coatings with Layered Silicates for Enhanced Corrosion Resistance and Mechanical Properties

Description: The new nickel/layered silicate nanocomposites were electrodeposited from different pHs to study the influence on the metal ions/layered silicate plating solution and on the properties of the deposited films. Nickel/layered silicate nanocomposites were fabricated from citrate bath atacidic pHs (1.6−3.0), from Watts’ type solution (pH ~4-5), and from citrate bath at basic pH (~9). Additionally, the new nickel/molybdenum/layered silicate nanocomposites were electrodeposited from citrate bath at pH 9.5. The silicate, montmorillonite (MMT), was exfoliated by stirring in aqueous solution over 24 hours. The plating solutions were analyzed for zeta potential, particle size, viscosity, and conductivity to investigate the effects of the composition at various pHs. The preferred crystalline orientation and the crystalline size of nickel, nickel/layered silicate, nickel/molybdenum, and nickel/molybdenum/layered silicate films were examined by X-ray diffraction. The microstructure of the coatings and the surface roughness was investigated by scanning electron microscopy and atomic force microscopy. Nickel/molybdenum/layered silicate nanocomposites containing low content of layered silicate (1.0 g/L) had increase 32 % hardness and 22 % Young’s modulus values over the pure nickel/molybdenum alloy films. The potentiodynamic polarization and electrochemical impedance measurements showed that the nickel/molybdenum/layered silicate nanocomposite layers have higher corrosion resistance in 3.5% NaCl compared to the pure alloy films. The corrosion current density of the nickel/molybdenum/layered silicate nanocomposite composed of 0.5 g/L MMT is 0.63 µA·cm-2 as compare to a nickel/molybdenum alloy which is 2.00 µA·cm-2.
Date: August 2014
Creator: Tientong, Jeerapan
Partner: UNT Libraries