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Development of an enantioselective two-dimensional liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry method for the analysis of methylsulfonyl polychlorinated biphenyls in tissue extractsCooper, Victoria Irene Unknown Date
No description available.
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Dynamic variation of hydrogen dilution during hot-wire chemical vapour deposition of silicon thin filmsTowfie, Nazley January 2013 (has links)
It has been debated that among all the renewable energy alternatives, only solar energy offers sufficient resources to meet energy demands. Silicon thin film solar cells are at the frontier of commercial solar technology. Hot wire chemical vapour deposition (HWCVD) is the technique of choice for silicon thin film deposition due to the absence of ion bombardment and its independence toward geometry or electromagnetic properties of the substrate, as seen by plasma enhanced chemical vapour deposition (PECVD). With the implementation of nanostructures in a
multi-band gap tandem solar cell, considerable improvement has been achieved over the single junction solar cells. Defect assisted tunnelling processes at the junctions between individual solar cells in a tandem structure solar cell largely affect the efficiency of these solar cells. In this contribution, the investigation toward the improvement of silicon thin films for tandem solar cell application is initiated. This study reports on the effects of hydrogen dilution and deposition time on six silicon thin films deposited at six specific deposition regimes. The thin film properties are investigated via X-Ray diffraction analysis, Raman spectroscopy, Fourier transform infra-red spectroscopy, elastic recoil detection analysis, scanning and transmission electron microscopy and UV-visible spectroscopy. This investigation revealed the dominating etching effect of atomic hydrogen with
the increase in hydrogen dilution and a bonded hydrogen content (CH) exceeding 10 at.% for each of the six thin films. The optically determined void volume fraction and static refractive index remain constant, for each thin film, with the change in CH. A new deposition procedure, utilising the deposition conditions of the previously investigated thin films, is performed by HWCVD to deposit two silicon thin films. This deposition procedure involved either increasing (protocol 1) or decreasing (protocol 2) hydrogen dilution during deposition. Structural and optical variation with depth was observed for the dynamically deposited silicon thin films, with nano-voids existing across the entire cross section and bond angle variations which are indicative of good structural order. The optical absorption curves differ for the two silicon thin films whereas the optical density remains constant for both. / >Magister Scientiae - MSc
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Gold(I)-Catalyzed Synthesis of Polycyclic Frameworks Related to Terpenes: Selective Divergent Synthesis of Fused CarbocyclesBarabe, Francis 07 November 2013 (has links)
Gold catalysis has become an important tool to achieve highly chemoselective p-acid activation. Exceptional reactivity and selectivity are often encountered under mild reaction conditions. These properties have made gold(I) complexes suitable catalysts for tremendous applications in the total synthesis of natural products. The first chapter will highlight a number of total syntheses using gold catalysis as a key step.
The second chapter will cover our application of the gold(I)-catalyzed 6-endo-dig carbocyclization for the synthesis of bridgehead-substituted scaffolds and its use toward the synthesis of PPAP natural products. This research has opened our eyes to the utility of biphenylphosphine ligands, particularly JohnPhos, in gold(I)-catalysis.
The reactivity and selectivity exhibited by gold(I) complexes is modulated by the nature of the ancillary ligand. Recent research rationalizes the impact of these ligands on the divergent reactivity observed between cationic and carbenoid intermediates. Our desire to favor the 6-endo-dig pathway has led us toward the discovery of another example of the diagonal reactivity that NHC carbene and biphenylphosphine ligands can bring to gold(I)-catalysis. Chapter three will explain the development of a selective gold-catalyzed synthesis of fused carbocycles
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Our selective divergent synthesis of fused carbocycles, combined with the Diels–Alder reaction, has brought new synthetic opportunities. Chapter four will describe our approach toward the synthesis of various polycyclic diterpene-related frameworks. Starting with a unique linear precursor, we have developed a new “one-pot” process for the synthesis of three different polycyclic compounds related to the terpenoid family. The facile modulation of the linear precursor and the use of different dienophiles during the Diels–Alder reaction could enable the synthesis of diverse polycyclic analogues based on three principal frameworks.
The gold(I)-catalyzed synthesis of fused carbocycles reached some limitations during our study. Regioselective control was found to be substantially more challenging, with terminal alkynes or alkynes bearing a sterically and electronically neutral methyl substituent. In chapter five, we will discuss how the complementarity of silver(I) catalysis to gold(I) catalysis enabled the selective divergent synthesis of three different fused carbocycles from a unique precursor. Moreover, copper(I) catalysis has given access to the 6-endo-dig pathway on terminal alkynes without the formation of a vinylidene intermediate.
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Development of an enantioselective two-dimensional liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry method for the analysis of methylsulfonyl polychlorinated biphenyls in tissue extractsCooper, Victoria Irene 06 1900 (has links)
An enantioselective heart-cut two-dimensional liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry method was developed for the analysis of 25 methylsulfonyl polychlorinated biphenyl metabolites in tissue extracts. Enantioseparation was achieved for 9 out of the 10 chiral analytes in less than 91 minutes, improving upon previous gas chromatography-based methods. Use of a pyrenyl-ethyl silica column in the first dimension enabled separation of all but two pairs of isobaric analytes. Limits of detection of 0.01 to 1.73 ng on-column were achieved. The precision and accuracy were within acceptable limits, but poor sensitivity was achieved for several meta-methylsulfonyl-substituted congeners. Despite this limitation, the method was successfully applied to the analysis of Greenland sledge dog (Canis familiaris) plasma and adipose tissue extracts. Concentration and enantiomer fraction data are presented. None of the target analytes were detected in Norwegian glaucous gull (Larus hyperboreus) plasma extracts.
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New Techniques for Sample Preparation in Analytical Chemistry : Microextraction in Packed Syringe (MEPS) and Methacrylate Based Monolithic Pipette TipsAltun, Zeki January 2008 (has links)
Sample preparation is often a bottleneck in systems for chemical analysis. The aim of this work was to investigate and develop new techniques to address some of the shortcomings of current sample preparation methods. The goal has been to provide full automation, on-line coupling to detection systems, short sample preparation times and high-throughput. In this work a new technique for sample preparation that can be connected on-line to liquid chromatography (LC) and gas chromatography (GC) has been developed. Microextraction in packed syringe (MEPS) is a new solid-phase extraction (SPE) technique that is miniaturized and can be fully automated. In MEPS approximately 1 mg of sorbent material is inserted into a gas tight syringe (100-250 μL) as a plug. Sample preparation takes place on the packed bed. Evaluation of the technique was done by the determination of local anaesthetics in human plasma samples using MEPS on-line with LC and tandem mass spectrometry (MS-MS). MEPS connected to an autosampler was fully automated and clean-up of the samples took about one minute. In addition, in the case of plasma samples the same plug of sorbent could be used for about 100 extractions before it was discarded. A further aim of this work was to increase sample preparation throughput. To do that disposable pipette tips were packed with a plug of porous polymer monoliths as sample adsorbent and were then used in connection with 96-well plates and LC-MS-MS. The evaluation of the methods was done by the analysis of local anaesthetics lidocaine and ropivacaine, and anti-cancer drug roscovitine in plasma samples. When roscovitine and lidocaine in human plasma and water samples were used as model substances, a 96-plate was handled in about two minutes. Further, disposable pipette tips may be produced at low cost and because they are used only once, carry-over is eliminated.
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Application of mass spectrometry in enzyme deficiency assay for newborn screening purpose /Wang, Ding, January 2006 (has links)
Thesis (Ph. D.)--University of Washington, 2006. / Vita. Includes bibliographical references (leaves 137-143).
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Beiträge zur Weiterentwicklung der Olefinmetathese Naturstoffsynthese und neue Katalysatoren /Buschmann, Nicole. Unknown Date (has links) (PDF)
Techn. Universiẗat, Diss., 2002--Berlin.
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Natur- und Wirkstoffsynthese: (+)-Astrophylline durch Ringumlagerungsmetathese potentielle makrocyclische Metalloproteaseinhibitoren durch RCM /Schaudt, Marco. Unknown Date (has links) (PDF)
Techn. Universiẗat, Diss., 2003--Berlin.
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Photoreaktionen tricyclischer Cyclopropylketone Aufbau von Polyquinanen und analoger Ringsysteme /Tzvetkov, Nikolay. Unknown Date (has links) (PDF)
Universiẗat, Diss., 2005--Bielefeld. / Erscheinungsjahr an der Haupttitelstelle: 2004.
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Dynamic variation of hydrogen dilution during hot-wire chemical vapour deposition of silicon thin filmsTowfie, Nazley January 2013 (has links)
>Magister Scientiae - MSc / This study reports on the effects of hydrogen dilution and deposition time on six silicon thin films deposited at six specific deposition regimes. The thin film properties are investigated via X-Ray diffraction analysis, raman spectroscopy, fourier transform infra-red spectroscopy, elastic recoil detection analysis, scanning and transmission electron microscopy and UV-visible spectroscopy. This investigation revealed the dominating etching effect of atomic hydrogen with
the increase in hydrogen dilution and a bonded hydrogen content (CH) exceeding 10 at.% for each of the six thin films. The optically determined void volume fraction and static refractive index remain constant, for each thin film, with the change in CH
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