<p>Sutherlandia frutescens (tribe Galegeae, Fabaceae), is a popular medicinal plant traditionally used in South Africa. In 2000, a company called Phyto Nova (Pty) Ltd. initiated large-scale cultivation and contract manufacturing of tablets, made from the powdered herb (i.e. thin stems and leaves). Most of these commercial Sutherlandia solid dosage forms are made from the dried leaf powder but recently a new product, viz. Promune&trade / capsules, made from a freeze-dried aqueous extract, came on the market and was claimed to be &ldquo / better&rdquo / as it mimics the traditional tea. However, the pharmaceutical quality and stability of these preparations have not yet been investigated. The objectives of this study were firstly, to develop a validated stability-indicating HPLC assay for sutherlandioside B (SU-B) / secondly, to compare the SU-B levels in the two commercially available Sutherlandia products viz, the Phyto Nova Sutherlandia SU1&trade / tablet and the Promune&trade / capsule, and, thirdly, to determine the effect of elevated temperature and humidity as well as acid hydrolysis on the SU-B levels in these two products.</p>

In this experimental investigation, the tensile creep behavior of commercial-purity molybdenum sheet at temperatures between 1300°C and 1700°C is critically evaluated, based upon experimental creep testing and microstructural characterizations. The high-temperature properties of molybdenum are of interest because there are many applications in which molybdenum and molybdenum alloys are used at elevated temperatures. Understanding of the creep mechanisms and the constitutive relations between stress and strain at elevated temperatures is needed in order to determine if molybdenum is an appropriate choice for a given high-temperature design application and to accurately predict its creep life. The creep behavior of two commercially-available grades of molybdenum was determined using short-term creep tests (1/2 to 14 hours) at slow to moderate true-strain rates of 10⁻⁶ to 10⁻⁴ s⁻¹ and temperatures between 1300°C and 1700°C. High-temperature, uniaxial tensile testing was used to produce data defining the relationship between tensile creep strain-rate and steady-state flow stress at four temperatures: 1340°C, 1440°C, 1540°C, 1640°C. Microstructural changes that occurred during creep testing were evaluated and compared to changes resulting from elevated temperature exposure alone. Mechanisms for dynamic abnormal grain growth that occurred during creep testing and the causes of the microstructural changes that occurred as a function of temperature are discussed. / text

<p>Sutherlandia frutescens (tribe Galegeae, Fabaceae), is a popular medicinal plant traditionally used in South Africa. In 2000, a company called Phyto Nova (Pty) Ltd. initiated large-scale cultivation and contract manufacturing of tablets, made from the powdered herb (i.e. thin stems and leaves). Most of these commercial Sutherlandia solid dosage forms are made from the dried leaf powder but recently a new product, viz. Promune&trade / capsules, made from a freeze-dried aqueous extract, came on the market and was claimed to be &ldquo / better&rdquo / as it mimics the traditional tea. However, the pharmaceutical quality and stability of these preparations have not yet been investigated. The objectives of this study were firstly, to develop a validated stability-indicating HPLC assay for sutherlandioside B (SU-B) / secondly, to compare the SU-B levels in the two commercially available Sutherlandia products viz, the Phyto Nova Sutherlandia SU1&trade / tablet and the Promune&trade / capsule, and, thirdly, to determine the effect of elevated temperature and humidity as well as acid hydrolysis on the SU-B levels in these two products.</p>

A concentração do gás carbônico (CO2) tem aumentado nas últimas décadas, devido principalmente à queima de combustíveis fósseis. Como consequência, admite-se que haverá gradual aumento da temperatura atmosférica em nível global. A soja é importante planta agrícola em todo o mundo, consumida na alimentação humana e de animais domésticos. O presente trabalho compõe-se de dois capítulos, o primeiro versando sobre o efeito da concentração de gás carbônico e da temperatura sobre vários parâmetros bioquímicos e o segundo, sobre a composição da cera foliar cuticular de uma variedade de soja. O capítulo I trata da composição química dos grãos e do teor de ceras foliares de plantas da cultivar \'MG/BR-46 Conquista\' crescendo em câmaras de topo aberto sob duas condições de CO2 (380ppm ambiente e 800ppm elevado) e duas condições de temperatura (ambiente e elevada [+5°C]). Foram coletados dados de 6 coletas ao longo de 105 dias de desenvolvimento da planta. As plantas crescidas em altas concentrações de CO2 aumentaram a biomassa seca da folha, caule, raiz e frutos, além do número de sementes; temperaturas elevadas estimularam a senescência precoce. A floração foi antecipada sob condição de CO2 elevado. Entre os carboidratos dos grãos, os teores de amido, frutose e mio-inositol tenderam a diminuir, enquanto os de sacarose, glicose e rafinose aumentaram. O incremento de CO2 acelerou a translocação de açúcares, enquanto e o da temperatura desacelerou. O teor de óleo e a composição dos ácidos graxos foram afetados diretamente pela elevada temperatura, com redução do teor de ácidos poliinsaturados. A associação de temperatura e CO2 elevados reduziu ainda mais o teor de ácidos graxos poliinsaturados. Os teores de proteínas solúveis em geral não apresentaram diferenças significativas por efeito do acoplamento, embora o teor de nitrogênio total tenha aumentado por efeito do tratamento por temperatura elevada. O teor de clorofilas foliares diminuiu por efeito dos tratamentos e o teor de cera foliar foi alterado ao longo do tempo. Conclui-se que as elevações de CO2 e temperatura, previstas para um futuro próximo, poderão ter o efeito de aumentar a produção de óleo por plantas de \'MG/BR-46 Conquista\', devido ao aumento no número de sementes por planta e elevação do teor de óleo. O capítulo II trata do teor da cera e a identificação dos componentes da cera foliar cuticular, por extração por lavagens superficiais das folhas com diclorometano, separação das classes de constituintes da cera por cromatografia em camada delgada e análise das frações por cromatografia a gás acoplada a espectrometria de massas. Os principais constituintes da cera foram os ésteres, seguidos de n-alcanos. O éster mais abundante foi o eicosanoato de octadecila (C38). Os alcanos principais foram o hentriacontano (C31) e o nonacosano (C29). Outros componentes detectados foram álcoois primários, ácidos graxos, hidroxiácidos graxos, álcoois triterpênicos e esteróis. O principal n-álcool graxo primário foi o octacosanol. Os triterpenos alcoólicos detectados foram &alpha;- e &beta;-amirinas, lupeol, germanicol e 12,20(29)-lupadien-3-ol. Os ácidos graxos variaram no intervalo C15-C28. Os esteroides detectados foram estigmasterol, campesterol, sitosterol e estigmastanol, com predominância do primeiro / The concentration of carbon dioxide (CO2) has increased in the last decades, due mainly to the combustion of fossil fuels. A gradual increase of the global temperature is expected as a consequence. Soybean is an important crop in most countries, being consumed either as human or domestic animals food. The present work is composed of two chapters, the first dealing with the effect of the concentration of carbon dioxide and temperature on several biochemical parameters, and the second on the composition of the foliar cuticular wax of a variety of soybean plant. Chapter one deals with the chemical composition of soybeans and the leaf wax contents of soybean variety \'MG/BR-46 Conquista\', growing in open top chambers under two conditions of CO2 (380 ppm - ambient, and 800 ppm - elevated) and two temperature conditions (ambient and elevated [+5°C]). The data were obtained from six collections along 105 days of experimentation. Elevated CO2 increased the dry weight of leaf, stem, root and fruit, as well as the number of seeds; elevated temperature stimulated early senescence. Early flowering occurred under elevated CO2. Among the grain carbohydrates, the contents of starch, fructose and myo-inositol decreased, whereas those of sucrose, glucose and raffinose increased. The effect of elevated CO2 and temperature accelerated the sugar translocation while that of elevated temperature slowed it down. The oil content and fatty acid composition were affected directly by the elevated temperature, a reduction of the content of polyunsaturated fatty acids having been observed. The coupling of elevated CO2 and temperature reduced even further the content of polyunsaturated acids. In general, the content of soluble proteins did not change significantly by the effect of treatment associating temperature and CO2, although the total nitrogen content increased by the effect of elevated temperature. The content of leaf chlorophylls decreased and the foliar wax content changed with time. It is concluded that the increase of temperature and atmospheric CO2, expected to take place in the near future, will possibly have the effect of increasing the production of oil by plants of \'MG/BR-46 Conquista\', due to the increase of the number of seeds per individual and the increase of the seed oil content. Chapter two deals with the concentration and identification of the components of the foliar cuticular wax of the soybean variety \'MG/BR-46 Conquista\', by means of surface washings of the leaves with dichloromethane, separation of the classes of wax constituents by thin layer chromatography and analysis of the fractions by gas chromatography coupled with mass spectrometry. The main constituents of the wax were esters, followed by n-alkanes. The main ester constituent was eicosanoate of octadecyl (C38). The main alkanes were n-hentriacontane (C31) and n-nonacosane (C29). Other constituents detected were primary alcohols, fatty acids, hydroxyacids, triterpene alcohols and sterols. The main n-primary alcohol was octacosanol. The triterpene alcohols detected were &alpha;- e &beta;-amyrins, lupeol, germanicol and 12,20(29)-lupadien-3-ol. The steroids detected were stigmasterol, campesterol, sitosterol and stigmastanol, with predominance of stigmasterol

Le procédé industriel TEL permet de fabriquer de la laine de verre en fibrant du verre en fusion. La pièce principale de ce procédé est « l’assiette de fibrage », qui est soumise à de nombreuses contraintes en service (oxydation, corrosion, érosion et fluage). Elle est actuellement élaborée par fonderie et réalisée en superalliage base nickel ou base cobalt. Fibrer de nouveaux types de verre impliquant des températures de travail plus élevées nécessite un nouveau type de superalliage. Le chrome est un candidat idéal pour être l’élément principal d’une assiette de par sa haute température de fusion et de par la résistance qu’il apporte aux superalliages usuels contre l’oxydation et la corrosion grâce à la formation d'une couche de chromine continue à la surface des alliages. Durant ces travaux de doctorat, une centaine d'alliages base chrome de compositions différentes ont été réalisés par fonderie. La découpe de tels alliages a montré un fort manque de ductilité à température ambiante. Des tests de dureté à température ambiante, d'oxydation et de fluage à haute température ont été menés. Une caractérisation métallographique complète a été réalisée sur ces alliages (DRX, MEB, microsonde de Castaing) à l'état brut de coulée, après recuit isotherme et après oxydation isotherme. L’étude approfondie d’alliages simples a permis de découvrir des compositions permettant de régler le problème de fragilité. Les alliages ont ensuite été complexifiés avec l'ajout d'autres éléments, permettant alors de corriger certains problèmes inhérents à des alliages à base de chrome. / The TEL process is used to produce glass wool at very high temperature. The main piece of this process is the “spinner”, which is exposed, in service, to numerous operating constraints (oxidation, corrosion, erosion and creep). This spinner is currently made of cobalt- or nickel-based superalloys and is fabricated by casting. To fiberize new glasses or to increase the current maximal fiberizing temperature, a new type of superalloy is required. Chromium is an ideal candidate to be the principal element of a new superalloy because of its very high melting point and its ability to develop a chromia protective scale against oxidation and corrosion at high temperature, reason for which it is usually added to many classical superalloys. During this Ph.D work, the synthesis and the study of more than a hundred of chromium-based alloys with different chemical compositions was done by casting. These alloys are brittle at room temperature during their cutting. Laboratory tests of hardness at room temperature, oxidation and 3 points flexural creep at high temperature were performed. Metallographic characterisations were carried out (XRD, SEM, EPMA) on all alloys in their as-cast state, after isothermal annealing or isothermal oxidation. The detailed study of simple alloys permitted to discover some compositions removing the brittleness problem of these alloys. Then, the enrichment of the composition of the alloys by addition of new elements, allowed to correct some inherent problems of chromium-based alloys.

Magister Pharmaceuticae - MPharm

This thesis deals with lead-acid battery, its parameters and temperature behaviour of this electro-chemical source of power. In the theory section, types of batteries are presented, followed by their primary parameters and electro-chemical reactions, which take part in battery cells. This section also contains information about charging stages, detailed description of each battery part, used materials, construction of the battery and degradation processes caused by battery operation. The practictal section of this thesis offers a measurement scheme for automated measuring workstation. Furthermore, the practical section presents results of measurements on parameters of chosen lead-acid battery types, it also contains long-term deep battery cycling and measurements under elevated temperatures. Detailed comparison of measurements results and datasheet values is included. Conclusion sums up parameters of chosen lead-acid battery types and their feasibility for further usage in power backuping.

This diploma thesis deals with monitoring of the influence of temperature on the properties of lithium-ion batteries, especially on the safety and capacity of selected batteries. Chapters 1 and 2 contain a literature review on the subject, describing electrochemical energy sources, especially secondary accumulators, mainly lithium-ion cells. Furthermore, the safety and degradation processes of lithium-ion batteries are discussed and the third chapter describes the design of experiments, realization and outputs of these experiments.

This dissertation contains the following sections. Chapter 1 contains a detailed description of the theory of thin layer chromatography (TLC). Chapter 2 describes the benefits and practical considerations of elevated temperatures in liquid chromatography (LC). The porous graphitic carbon (PGC) I modified as part of my work is often used in elevated temperature LC. Chapter 3 shows a thermodynamic analysis of chromatographic retention at elevated temperature, and Chapter 4 contains a closer look at the van 't Hoff equation in LC and how it can be used in retention modeling. In Chapter 5, I describe a new procedure for microfabricating TLC plates that avoids the volume/feature distortions that occurred in our first microfabrication. The primary advance of this work was the priming of the carbon nanotube (CNT) forests with chemical vapor deposition (CVD) carbon and atomic layer deposition (ALD) alumina, which permitted effective ALD-like deposition of SiO2. Chapter 6 describes advancements in the microfabrication process of TLC, which excluded the use of the CVD carbon and Al2O3 coating as described in Chapter 5. The use of ozone, to lightly oxidize the CNT surface, primed the material for direct ALD deposition. Chapter 7 gives a detailed surface analysis of the microfabrication process up to and including the CNT forest. It was noticed that a channeling effect was present during Rutherford backscattering analysis of the CNTs. Additionally, characterization of CNTs using time-of-flight secondary ion mass spectrometry in the negative ion mode showed an odd-even effect for a homologous series of carbon, where the even moieties had a stronger signal. Chapter 8 describes the functionalization of PGC with di-tert-amyl peroxide (DTAP) and its effect on increasing the chromatographic performance as seen by a reduction in the tailing factors of test analytes. Chapter 9 -- 13 are detailed X-ray photoelectron analyses of the thin films and CNTs used in producing microfabricated TLC plates.

My work has focused on a variety of different types of diamond-based, core-shell particles. These particles are formed with inert cores and poly(allylamine)/nanodiamond shells. Their intended purpose is to form an LC stationary phase that is stable from pH 1 – 14 and at elevated temperatures. At the beginning of my studies, the particles that had been made in the Linford laboratory were pH stable, but irregular and had poor mechanical stability. Since that time, I have worked to improve the particles by using more spherical zirconia and carbon cores, and I have improved their mechanical stability via chemical crosslinking with epoxides. I have performed van Deemter and van’t Hoff analyses to understand the properties of these columns. Efficiencies greater than 100,000 N/m are routinely achieved with these carbon/nanodiamond-based phases. In addition I contributed to two patents that show innovations in diamond functionalization. My contributions involved reduction of an oxidized diamond surface with LiAlH4 prior to functionalization with isocyanates. I also wrote some application notes for the Flare mixed-mode column, which was recently introduced to the market and contains particles comprised of a carbon core and a polymer/nanodiamond shell. These application notes show the gradient separations of four essential oils (lavender, melaleuca, peppermint and eucalyptus), and the isocratic separations of various triazine herbicides and a mixture of β2-agonists and amphetamines.This dissertation contains the following sections. Chapter 1 is a review of liquid chromatographic history and theory. It also includes a history of the use of diamonds in liquid chromatography. Chapter 2 is a study on a glassy carbon core - polymer/nanodiamond shell particle made in our laboratory. Stability studies at pH 11.3 and 13 were performed and different analytes were retained and/or separated on the column. Chapter 3 is a study performed on the Flare mixed-mode column. Separations of tricyclic antidepressants, β2-andrenergic receptor agonists, and linear chain alkylbenzenes were demonstrated with this phase. Van Deemter and van’t Hoff studies were also performed to probe the efficiency and selectivity of this column with different classes of analytes. Chapter 4 chronicles, via SEM and van Deemter analysis, the improvements that have taken place in our column after many iterations of improved synthetic methods and new materials. These include better particle uniformity, particle stability, and column efficiency. Three different carbon cores were analyzed, each better than the previous one. Appendices 1 – 6 are application notes published by Diamond Analytics of β2-andrenergic receptor agonists and amphetamines, triazine herbicides, and lavender, melaleuca, eucalyptus and peppermint essential oils. Appendices 7 and 8 are patents that contain ideas and research contributed by the author.