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Development and Validation of Methods for Characterization of Multi-Component Systems in Preparative LC / Utveckling och Validering av Metoder för Karaktärisering av Flerkomponentsystem vid Preparativ VätskekromatografiArnell, Robert January 2006 (has links)
<p>This thesis concerns the development and validation of methods for characterization of multi-component preparative LC systems. Measurements of competitive adsorption isotherms are performed to gain detailed information about the interactions inside the chromatography column. This information increases our understanding of the separation process and makes it possible to perform computer simulations and numerical optimizations to find optimal operating conditions.</p><p>The methods under focus are called “the tracer-pulse method”, “the inverse method”, and “the inverse method on plateaus”. They are extensions of existing methods, with new experimental and numerical procedures to enable rapid and accurate multi-component adsorption isotherm determination. In the validation it was shown that they can produce results agreeing with traditional methods and that the acquired adsorption isotherm parameters can be used in simulations to accurately predict the outcome of preparative LC separations.</p><p>The methods were used to characterize several complex LC systems and two phenomena were discovered and theoretically treated: 1) The presence of invisible deformed peaks in single-component systems. 2) Peak deformations encountered with modern chiral stationary phases, caused by strongly adsorbed eluent additives. The latter type of deformation was highly tuneable and it was possible to adjust the enantiomer peak shapes so that the peaks tailed in opposite directions with the sharp sides in between, yielding baseline resolution at remarkably high sample loads.</p><p>In a final applied study both the LC-based perturbation peak method and a biosensor method based on surface plasmon resonance (SPR) were used for the first time for detailed characterization of chiral drug-protein interactions. The fundamental properties of the two very different methods were compared and it was found that the LC method is more suitable for multi-component analysis and that the SPR method is more suitable for stronger interactions.</p>
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Advanced low temperature metal hydride materials for low temperature proton exchange membrane fuel cell applicationNtsendwana, Bulelwa January 2010 (has links)
<p>Energy is one of the basic needs of human beings and is extremely crucial for continued development of human life. Our work, leisure and our economic, social and physical welfare all depend on the sufficient, uninterrupted supply of energy. Therefore, it is essential to provide adequate and affordable energy for improving human welfare and raising living standards. Global concern over environmental climate change linked to fossil fuel consumption has increased pressure to generate power from renewable sources [1]. Although substantial advances in renewable energy technologies have been made, significant challenges remain in developing integrated renewable energy systems due primarily to mismatch between load demand and source capabilities [2]. The output from renewable energy sources such as photo-voltaic, wind, tidal, and micro-hydro fluctuate on an hourly, daily, and seasonal basis. As a result, these devices are not well suited for directly powering loads that require a uniform and uninterrupted supply of input energy.</p>
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Development and Validation of HPLC Methods for Analytical and Preparative PurposesLindholm, Johan January 2004 (has links)
This thesis concerns the development and validation of high performance liquid chromatography (HPLC) methods aimed for two industrially important areas: (i) analysis of biotechnological synthesis and (ii) determination of adsorption isotherm parameters. There is today a lack of detailed recommendations for analytical procedures in the field of biotechnological production of drugs. Therefore, guidelines were given for analytical development and validation in this field; the production of 9α-hydroxyprogesterone was used as model. In addition, a rapid method using HPLC coupled with diode-array-detection (DAD) and mass spectrometry (MS), was developed for the preliminary identification and quantification of the product. In addition, requirements and recommendations were developed for the selection of the internal standard and for its inclusion in the process liquid. By using this approach the precision and accuracy of the quantitative method were considerably improved. Preparative chromatography is a powerful separation method for the purification of pure compounds from more or less complex sample mixtures. One such mixture can be the process liquid from a fermentation, another example can be a racemic mixture of compounds whose enantiomeric constituents must be isolated. Computer-assisted modeling can be used to optimize preparative chromatography. However, competitive adsorption isotherm parameters are required as input data for the computer simulations. In this thesis, a new injection technique, based on a firm theoretical basis, was developed for the peak perturbation (PP) method allowing the determination of binary competitive adsorption isotherm parameters from a broad concentration range. With the new method the determination of adsorption isotherm parameters from a quaternary mixture could be done for the first time. The profiles simulated with these parameters showed excellent agreement with the corresponding experimental profiles, validating the accuracy of the adsorption isotherm parameters derived by the new method.
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Development and Validation of Methods for Characterization of Multi-Component Systems in Preparative LC / Utveckling och Validering av Metoder för Karaktärisering av Flerkomponentsystem vid Preparativ VätskekromatografiArnell, Robert January 2006 (has links)
This thesis concerns the development and validation of methods for characterization of multi-component preparative LC systems. Measurements of competitive adsorption isotherms are performed to gain detailed information about the interactions inside the chromatography column. This information increases our understanding of the separation process and makes it possible to perform computer simulations and numerical optimizations to find optimal operating conditions. The methods under focus are called “the tracer-pulse method”, “the inverse method”, and “the inverse method on plateaus”. They are extensions of existing methods, with new experimental and numerical procedures to enable rapid and accurate multi-component adsorption isotherm determination. In the validation it was shown that they can produce results agreeing with traditional methods and that the acquired adsorption isotherm parameters can be used in simulations to accurately predict the outcome of preparative LC separations. The methods were used to characterize several complex LC systems and two phenomena were discovered and theoretically treated: 1) The presence of invisible deformed peaks in single-component systems. 2) Peak deformations encountered with modern chiral stationary phases, caused by strongly adsorbed eluent additives. The latter type of deformation was highly tuneable and it was possible to adjust the enantiomer peak shapes so that the peaks tailed in opposite directions with the sharp sides in between, yielding baseline resolution at remarkably high sample loads. In a final applied study both the LC-based perturbation peak method and a biosensor method based on surface plasmon resonance (SPR) were used for the first time for detailed characterization of chiral drug-protein interactions. The fundamental properties of the two very different methods were compared and it was found that the LC method is more suitable for multi-component analysis and that the SPR method is more suitable for stronger interactions.
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Transport Properties and Durability of LCP and FRP materials for process equipmentRömhild, Stefanie January 2010 (has links)
This thesis focuses on transport properties and durability of liquid crystalline polymers (LCP)and fibre reinforced plastics (FRP) with regard to application in industrial process equipment.In the first part of the study the possibility of using a thermotropic LCP of type Vectra A950as lining material for FRP process equipment was investigated. Its performance wascompared to that of a fluorinated ethylene propylene copolymer (FEP) with respect tochemical and permeation resistance. Transport property and chemical resistance data wereestablished for different types of LCP film (compression molded, uniaxially and biaxiallyoriented film) exposed to selected chemicals chosen to represent typical industrial processenvironments. Annealing of the LCP, which may reduce the disclination density and henceimprove the barrier properties, induced a crystallinity increase, but did not significantlyimprove the barrier and chemical resistance properties. Different surface treatments toincrease the bonding between the LCP and FRP were explored. The conclusion was that LCPhas potential to serve as lining material for FRP in contact with water, organic solvents andnon-oxidizing acid environments, although certain issues, such as jointing techniques, stillhave to be evaluated. The second part of the study focused on transport and long-termproperties of commercial thermoset and FRP materials for industrial process equipment inaqueous environments (50 – 95 °C, water activity 0.78 – 1, exposure time ≤ 1000 days). Thewater transport properties in different thermosets were related to their chemical structureusing the solubility parameter concept. The transport of water in the thermosets with differentchemical structures could be predicted from the water activity, regardless of the actual type ofionic or non-ionic solute in the solution. An empirical relationship, independent of boththermoset chemistry and temperature, was established to describe the water concentration inthe thermoset as a function of water activity and the water concentration in pure water. Inlong-term, the water concentration in the thermosets increased with exposure time. Thisseemed to be primarily related to stress relaxation processes induced by water absorption andcertain leaching effects. The effects of hydrolysis seemed to be small. The glass fibrereinforcement may to various extents affect the water transport properties by capillarydiffusion and additional absorption around fibre bundles. The extent of such processesseemed to depend on temperature, water activity and the type of thermoset and reinforcement.The present work may be a useful contribution to an increased understanding of water effectsand durability of FRP process equipment. However, open questions still remain for a morecomprehensive durability analysis. / QC20100629
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A comparison of the reactivity of different synthetic calcium carbonate minerals with arsenic oxyanionsMandal, Abhishek 14 January 2009
This study was conducted to determine how the structure and surface chemistry of bulk CaCO3 differs from that of nanometer-sized CaCO3 and then to determine rate, extent and mechanisms of As adsorption on various synthetic CaCO3 materials. Additionally, we sought to devise a chemical CaCO3 precipitate that approximates biogenic CaCO3. The bulk CaCO3 precipitation was performed by using a solution that was highly oversaturated so that large CaCO3 precipitates rapidly form. Two different methods were employed for the synthesis of nanometer size CaCO3 i) an in situ deposition technique and ii) an interfacial reaction (water in oil emulsion). Mineral characterization of all CaCO3 precipitates was done with Nitrogen Porosimetry (Brunauer Emmett Teller method), particle size analysis, X-ray diffraction and Fourier Transform Infrared/ Fourier Transform Raman spectroscopy. The principal objective of the research was to assess the overall reactivity of As(III) and As(V) with different synthetic CaCO3 minerals. This was accomplished by i) running adsorption isotherms (varying As concentration), ii) measuring pH envelopes (varying pH at a fixed concentration) and iii) kinetic experiments (varying reaction time). Also, electrophoretic mobility experiments were performed in the presence of As(III) and As(V), and these studies revealed that As(III) forms stronger inner-sphere complexes with CaCO3 than As(V). Also, it was found that nanometer-sized CaCO3 prepared via deposition formed stronger inner-sphere complexes with As oxyanions (q = 5.26 µmol/m2) compared to either nano-sized CaCO3 from interfacial reactions (q = 4.51 µmol/m2) or bulk CaCO3 (q = 4.39 µmol/m2).<p>
The PEG-based nano CaCO3 prepared by an in-situ deposition technique presents a novel and readily available synthesis route that can be used as proxy for the biogenic CaCO3 known to be present in many different environmental conditions. The results of this study suggest that CaCO3 can be used as a sorbent for As in groundwater.
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A comparison of the reactivity of different synthetic calcium carbonate minerals with arsenic oxyanionsMandal, Abhishek 14 January 2009 (has links)
This study was conducted to determine how the structure and surface chemistry of bulk CaCO3 differs from that of nanometer-sized CaCO3 and then to determine rate, extent and mechanisms of As adsorption on various synthetic CaCO3 materials. Additionally, we sought to devise a chemical CaCO3 precipitate that approximates biogenic CaCO3. The bulk CaCO3 precipitation was performed by using a solution that was highly oversaturated so that large CaCO3 precipitates rapidly form. Two different methods were employed for the synthesis of nanometer size CaCO3 i) an in situ deposition technique and ii) an interfacial reaction (water in oil emulsion). Mineral characterization of all CaCO3 precipitates was done with Nitrogen Porosimetry (Brunauer Emmett Teller method), particle size analysis, X-ray diffraction and Fourier Transform Infrared/ Fourier Transform Raman spectroscopy. The principal objective of the research was to assess the overall reactivity of As(III) and As(V) with different synthetic CaCO3 minerals. This was accomplished by i) running adsorption isotherms (varying As concentration), ii) measuring pH envelopes (varying pH at a fixed concentration) and iii) kinetic experiments (varying reaction time). Also, electrophoretic mobility experiments were performed in the presence of As(III) and As(V), and these studies revealed that As(III) forms stronger inner-sphere complexes with CaCO3 than As(V). Also, it was found that nanometer-sized CaCO3 prepared via deposition formed stronger inner-sphere complexes with As oxyanions (q = 5.26 µmol/m2) compared to either nano-sized CaCO3 from interfacial reactions (q = 4.51 µmol/m2) or bulk CaCO3 (q = 4.39 µmol/m2).<p>
The PEG-based nano CaCO3 prepared by an in-situ deposition technique presents a novel and readily available synthesis route that can be used as proxy for the biogenic CaCO3 known to be present in many different environmental conditions. The results of this study suggest that CaCO3 can be used as a sorbent for As in groundwater.
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Strukturuntersuchungen an Methan- und Kohlenstoffdioxid-Clathrat-Hydraten / Crystal structure analysis of methane- and carbon doixide clathrate hydrateKlapproth, Alice 29 October 2002 (has links)
No description available.
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Advanced low temperature metal hydride materials for low temperature proton exchange membrane fuel cell applicationNtsendwana, Bulelwa January 2010 (has links)
<p>Energy is one of the basic needs of human beings and is extremely crucial for continued development of human life. Our work, leisure and our economic, social and physical welfare all depend on the sufficient, uninterrupted supply of energy. Therefore, it is essential to provide adequate and affordable energy for improving human welfare and raising living standards. Global concern over environmental climate change linked to fossil fuel consumption has increased pressure to generate power from renewable sources [1]. Although substantial advances in renewable energy technologies have been made, significant challenges remain in developing integrated renewable energy systems due primarily to mismatch between load demand and source capabilities [2]. The output from renewable energy sources such as photo-voltaic, wind, tidal, and micro-hydro fluctuate on an hourly, daily, and seasonal basis. As a result, these devices are not well suited for directly powering loads that require a uniform and uninterrupted supply of input energy.</p>
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Biogeochemical DefluoridationEvans-Tokaryk, Kerry 09 June 2011 (has links)
Fluoride in drinking water can lead to a crippling disease called fluorosis. As there is no cure for fluorosis, prevention is the only means of controlling the disease and research into fluoride remediation is critical. This work begins by providing a new approach to assessing fluoride remediation strategies using a combination of groundwater chemistry, saturation indices, and multivariate statistics based on the results of a large groundwater survey performed in a fluoride-contaminated region of India. From the Indian groundwater study, it was noted that one technique recommended for defluoridation involved using hydrous ferric oxide (HFO) as a solid phase sorbent for fluoride. This prompted investigation of bacteriogenic iron oxides (BIOS), a biogenic form of HFO, as a means of approaching bioremediation of fluoride. Batch sorption experiments at ionic strengths ranging from 0.001 to 0.1 M KNO3 and time course kinetic studies with BIOS and synthetic HFO were conducted to ascertain total sorption capacities (ST), sorption constants (Ks), and orders of reaction (n), as well as forward (kf) and reverse (kr) rate constants. Microcosm titration experiments were also conducted with BIOS and HFO in natural spring water from a groundwater discharge zone to evaluate fluoride sorption under field conditions. This thesis contributes significant, new information regarding the interaction between fluoride and BIOS, advancing knowledge of fluoride remediation and covering new ground in the uncharted field of fluoride bioremediation.
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