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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
121

Crystallization of Parabens : Thermodynamics, Nucleation and Processing

Huaiyu, Yang January 2013 (has links)
In this work, the solubility of butyl paraben in 7 pure solvents and in 5 different ethanol-water mixtures has been determined from 1 ˚C to 50 ˚C. The solubility of ethyl paraben and propyl paraben in various solvents has been determined at 10 ˚C. The molar solubility of butyl paraben in pure solvents and its thermodynamic properties, measured by Differential Scanning Calorimetry, have been used to estimate the activity of the pure solid phase, and solution activity coefficients. More than 5000 nucleation experiments of ethyl paraben, propyl paraben and butyl paraben in ethyl acetate, acetone, methanol, ethanol, propanol and 70%, 90% ethanol aqueous solution have been performed. The induction time of each paraben has been determined at three different supersaturation levels in various solvents. The wide variation in induction time reveals the stochastic nature of nucleation. The solid-liquid interfacial energy, free energy of nucleation, nuclei critical radius and pre-exponential factor of parabens in these solvents have been determined according to the classical nucleation theory, and different methods of evaluation are compared. The interfacial energy of parabens in these solvents tends to increase with decreasing mole fraction solubility but the correlation is not very strong. The influence of solvent on nucleation of each paraben and nucleation behavior of parabens in each solvent is discussed. There is a trend in the data that the higher the boiling point of the solvent and the higher the melting point of the solute, the more difficult is the nucleation. This observation is paralleled by the fact that a metastable polymorph has a lower interfacial energy than the stable form, and that a solid compound with a higher melting point appears to have a higher solid-melt and solid-aqueous solution interfacial energy. It has been found that when a paraben is added to aqueous solutions with a certain proportion of ethanol, the solution separates into two immiscible liquid phases in equilibrium. The top layer is water-rich and the bottom layer is paraben-rich. The area in the ternary phase diagram of the liquid-liquid-phase separation region increases with increasing temperature. The area of the liquid-liquid-phase separation region decreases from butyl paraben, propyl paraben to ethyl paraben at the constant temperature. Cooling crystallization of solutions of different proportions of butyl paraben, water and ethanol have been carried out and recorded using the Focused Beam Reflectance Method, Particle Vision and Measurement, and in-situ Infrared Spectroscopy. The FBRM and IR curves and the PVM photos track the appearance of liquid-liquid phase separation and crystallization. The results suggest that the liquid-liquid phase separation has a negative influence on the crystal size distribution. The work illustrates how Process Analytical Technology (PAT) can be used to increase the understanding of complex crystallizations. By cooling crystallization of butyl paraben under conditions of liquid-liquid-phase separation, crystals consisting of a porous layer in between two solid layers have been produced. The outer layers are transparent and compact while the middle layer is full of pores. The thickness of the porous layer can reach more than half of the whole crystal. These sandwich crystals contain only one polymorph as determined by Confocal Raman Microscopy and single crystal X-Ray Diffraction. However, the middle layer material melts at lower temperature than outer layer material. / <p>QC 20130515</p> / investigate nucleation and crystallization of drug-like organic molecules
122

Quantitative measurements of temperature using laser-induced thermal grating spectroscopy in reacting and non-reacting flows

Lowe, Steven January 2018 (has links)
This thesis is concerned with the development and application of laser induced thermal grating spectroscopy (LITGS) as a tool for thermometry in reacting and non-reacting flows. LITGS signals, which require resonant excitation of an absorbing species in the measurement region to produce a thermal grating, are acquired for systematic measurements of temperature in high pressure flames using OH and NO as target absorbing species in the burned gas. The signal obtained in LITGS measurements appears in the form of a time-based signal with a characteristic frequency proportional to the value or the sound speed of the local medium. With knowledge of the gas composition, the temperature can be derived from the speed of sound measurement. LITGS thermometry using resonant excitation of OH in the burned gas region of in oxygen enriched CH4/O2/N2 and CH4/air laminar flames was performed at elevated pressure (0.5 MPa) for a range of conditions. Measurements were acquired in oxygen enriched flames to provide an environment in which to demonstrate LITGS thermometry under high temperature conditions (up to 2900 K). The primary parameters that influence the quality of LITGS signal were also investigated. The signal contrast, which acts as a marker for the strength of the frequency oscillations, is shown to increase with an increase in the burnt gas density at the measurement point. LITGS employing resonant excitation of NO is also demonstrated for quantitative measurements of temperature in three environments – a static pressure cell at ambient temperature, a non-reacting heated jet at ambient pressure and a laminar premixed CH4/NH3/air flame operating at 0.5 MPa. Flame temperature measurements were acquired at various locations in the burned gas close to a water-cooled stagnation plate, demonstrating the capability of NO-LITGS thermometry for measuring the spatial distribution of temperature in combustion environments. In addition, the parameters that in influence the local temperature rise due to LITGS were also investigated in continuous vapour flows of acetone/air and toluene/air mixtures at atmospheric conditions. Acetone and toluene are commonly targeted species in previous LITGS measurements due to their favourable absorption characteristics. Results indicate that LITGS has the potential to produce accurate and precise measurements of temperature in non-reacting flows, but that the product of the pump intensity at the probe volume and the absorber concentration must remain relatively low to avoid significant localised heating of the measurement region.
123

<b>Molecular investigation of the multi-phase photochemistry of environmental aquatic systems</b>

Maria V Misovich (17553087) 08 December 2023 (has links)
<p dir="ltr">The chemical constituents of terrestrial and atmospheric waters originate from biomass burning, fertilizer runoff, and anthropogenic activity, among other sources, and their multi-phase chemistry is complex. Sunlight plays an essential role in aquatic chemistry. Photosensitizers in terrestrial and atmospheric waters absorb light to form highly reactive species such as triplet excited carbon (<sup>3</sup>C*), hydroxyl radical (•OH), and singlet oxygen (<sup>1</sup>O<sub>2</sub>), driving the photochemical transformations of dissolved organic matter (DOM) in the aqueous phase. Of note, these reactive species transform DOM compounds that do not undergo direct photolysis. DOM frequently undergoes a change in optical properties following photochemical processing, with implications for air quality, water quality, and human and animal health. The presence of inorganic minerals, such as the fertilizer compound struvite, in terrestrial or atmospheric waters introduces further complexity and impacts the photochemical processes that occur. Simplified proxy systems are created in the laboratory to simulate aquatic photochemical processes and evaluate the formation and/or photodegradation of photoproducts. These mixtures typically consist of a representative organic carbon (OC) compound and a photosensitizer, along with struvite or another inorganic mineral.</p>

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