Spelling suggestions: "subject:"calorimetry."" "subject:"alorimetry.""
631 |
Optimalizace technologických vlastností cementových formovacích směsí / Optimalization of Technological Properties of Cement Sand MixturesBurianová, Klára January 2017 (has links)
The work deals with optimization of the technological properties of cement-sand mixtures. The main objective is to find the correct mixture of the individual components which contribute to the rapid solidification of the mixture, hence shorter dismantling. The content is also of a method of measuring and recording during the plasticity of the mixture. Also assessment of the velocity of hydration heat cement mixture in the initial stage of the solidification process in the course of the strength properties of the mixture. To assess these phenomena was used calorimetric method used for measuring hydration heat cement mixture. Further measurements plasticity mixtures and mechanical and physical methods for measuring the compressive strength with the help of a measuring instrument LRU-D.
|
632 |
Reologické vlastnosti cementových past s přídavkem amorfního SiO2 / Reological properties of cement pastes modified by amorphous SiO2Zimmermann, Štěpán January 2017 (has links)
The subject of this thesis are the rheological properties of cement paste with the addition of amorphous silicon dioxide. The basic rheological parameters are that describe the behavior of cement pastes in the fresh state. The work also included rheological tests including measurement principle and method of evaluation. Effect of mineral admixtures with high content of amorphous SiO2 is summarized the available scientific articles. In the experimental part, the effects of impurities with a high content of amorphous SiO2 on the rheological properties of fresh cement paste. It was tested by substitution of up to 10 % by weight of cement in the cement pastes mineral admixtures of different chemical composition, particle size and pozzolanic activity. Flow measurement was measured yield value, viscosity, and flow index. The stability of cement pastes was investigated oscillatory measurements. To complement the behavior pastes in the fresh state was determined by calorimetry. Test results were compared with those determined by reference samples and compared the effect of various ingredients.
|
633 |
Optimalizace postupu izolace a charakterizace amorfních PHB granulí / Optimisation of Isolation Procedure and Characterization of Amorphous PHB granulesKratochvíl, Zdeněk January 2017 (has links)
First artificial PHB granules were prepared under the terms of this thesis. The effect of used PHB solvent, ultrasonic bath temperature and time, solvent evaporation temperature and stabilizing agent nature was investigated using dynamic and electrophoretic light scattering. The most proper parameters were demonstrated at samples which were prepared by dissolving of PHB in chloroform, stabilizing with CTAB or lecithin, ultrasonifying at 35 °C followed by chloroform evaporating at 60 °C. Based on ATR-FTIR and Raman spectroscopy results, it was found out that PHB within the artificial granules were in crystalline form. The native PHB granules were isolated from Cupriavidus necator using either lysosyme, deoxyribonuclease and cell disruption by ultrasonification or digestion with alcalase, SDS and EDTA. Granules obtained by both isolation procedures were characterized by ATR-FTIR, Raman spectroscopy, light scattering techniques and DSC. According to the analyses results, the second mentioned procedure turned out to be more effective for obtaining the polymer in amorphous state. Furthermore, the polymer within granules recovered by using this procedure was thermally more stable. Last but not least, the native PHB granules samples were exposed to effect of acetone, lipase and sodium hypochlorite, assuming that polymer crystallinity should be increased by these chemicals in varying degrees. The highest degree of crystallinity was achieved after their treatment with lipase.
|
634 |
Morfologie polyamidu 12 a polyamidu 11 vzniklá za zvýšeného tlaku v kalorimetru / Morphology of Polyamide 12 and Polyamide 11 formed at overpressure and underpressureBělašková, Marie January 2017 (has links)
In this master thesis it was studied morphology of polyamide 12 (PA12), polyamide 11 (PA11) and their blends in the percent ratios 95/5, 75/25, 50/50, 25/75 and 5/95 formed at pressure 7 MPa in a calorimeter both after continual heating and cooling and after annealing and isothermal crystallization. Neat polyamides and blends were further characterized by thermogravimetric analysis, differential scanning calorimetry at atmospheric pressure, Fourier-transform infrared spectroscopy in attenuated total refection, and X-ray diffraction analysis. The increased pressure improved level of polyamide chains ordering in crystal lamellae. Thermal annealing improved especially ordering of PA12, isothermal crystallization led to considerable increase of crystallinity, whereas PA11-rich blends supported perfection of PA12 crystals. Partial transformation of - to -structure occurred in case of neat PA12 at high pressure, the change of the chain conformation into the closer one occurred in neat PA11 without transformation of the type of crystal structure.
|
635 |
Catalytic synthesis and decomposition of peroxycarboxylic acids / Synthèse catalytique et décomposition des acides peroxycarboliquesLeveneur, Sébastien 23 October 2009 (has links)
L'objectif de cette thèse fut de développer un process pour la production d'acide peroxycarbolique à partir du peroxyde d'hydrogène et d'un acide carboxylique dans un réacteur continu. Dans un premier temps, la stabilité des espèces peroxydées fut étudiée en utilisant une méthode d'analyse en direct (spectromètre de masse). Un effort particulier a été apporté pour trouver un catalyseur hétérogène ne provoquant pas la décomposition des espèces peroxydées et ayant une activité catalytique similaire à l'acide sulfurique. Un réacteur en continu en lit fixe a été construit en utilisant des résines échangeuses de cation. / The purpose of this thesis was to find a way to produce peroxycarboxylic acid from hydrogen peroxide and carboylic acid in a continuous reactor by using heterogeneous catalysts. In the first step the stability of peroxyde species xas studied by using an online analytic method (Mass spectrometer). One of the main challenge was to find a suitable solid acid catalyst, wich does no decompose the peroxyde species and can catalyze the reaction as sulfuric acid. A continuous fixed bed reactor was built by using caion exchange resins as a catalyst.
|
636 |
Development of Non-Amorphous Solid Dispersions for Poorly-Soluble Drugs Using a Novel Excipient and Hot Melt ExtrusionHwee Jing Ong (5930108) 16 January 2020 (has links)
<div>Drug solubility is a persistent challenge in pharmaceutical product development. The objective of this research is to develop a formulation/processing strategy by means of a biodendrimeric solid dispersion (BDSD) platform, for increasing the solubility and dissolution rate of poorly water-soluble drugs. The BSDS platform combines a novel type of excipient, referred to as DLB, with a new application of the hot melt extrusion (HME) process.</div><div><br></div><div>Four model compounds – phenytoin (PHT), griseofulvin (GSF), ibuprofen (IBU), and loratadine (LOR) – were used to evaluate the solubilization effect of an octenylsuccinate-modified dendrimer-like biopolymer (OS-DLB). Shake-flask solubility measurements show that OS-DLB exerts significant solubilizing effect when present at less than 0.2% in water. The presence of hydrophobic C<sub>8</sub> chains on OS-DLB creates the type of favorable nonpolar microenvironment necessary for producing a parallel liquid phase equilibrium responsible for the increase in the total amount of drug dissolved in aqueous media. The higher the hydrophobicity of the drug, the higher the observed solubilization effect. Isothermal titration calorimetry studies show that drug solubilization by OS-DLB occurs by means of entropy-driven interactions. These studies also show that the intermolecular interaction between IBU and OS-DLB in solution exhibits very small energy change upon mixing but a stronger effect on entropy. In comparison, the intermolecular interaction between the less hydrophobic GSF and OS-DLB have significant effects on both enthalpy and entropy. Consequently, in terms of solubilization enhancement, it was found that the interaction between IBU and OS-DLB is entropy-driven (more favorable), while in the case of GSF, the interacting molecules are arranged to maximize enthalpic interaction.</div><div><br></div><div>Based on the solubility studies, a formulation/processing approach for enhancing the dissolution rate of the model drugs was developed. The biopolymer serving as both carrier and solubilizing agent, was coprocessed with poloxamer, functioning as a processing aid, using hot melt extrusion (HME) as an enabling technology. The result is a non-amorphous solid dispersion, exhibiting high and long-lasting supersaturation upon dissolution. A 3-factor, 3-level Box-Behnken design was implemented to define the optimal design space for the formulation/extrusion process. The results obtained from multivariate data analysis (partial least squares and principal components analysis) and response surface modeling suggest that drug release performance of IBU BDSDs is strongly influenced by the processing variables, while maximum release of GSF from the BDSDs can be attained through selective combination of functional excipients.<br></div>
|
637 |
Protein interaction with polyelectrolytes and ligands: A structural and thermodynamic investigationYu, Shun 29 August 2017 (has links)
Der erste Teil dieser Arbeit untersucht die Ladungswechselwirkung zwischen Proteinen und Polyelektrolyten. Dabei wird die Bindung von Polyakrylsäure (PAA) als kurzes Modell-Polyelektrolyt an Humanalbumin (HSA) in einer umfassenden experimentellen und theoretischen Studie untersucht und sehr gute Übereinstimmung der Resultate konnte festgestellt werden. Die Computersimulationen in dieser Arbeit wurden von Xiao Xu im Rahmen seiner Promotion durchgeführt. Thermodynamische Daten wurden mit Hilfe von Isothermer Titrationskalorimetrie (ITC) gesammelt und strukturelle Untersuchungen wurden mit Hilfe von Neutronenkleinwinkelstreuung (SANS) durchgeführt. Die Analyse von Bindungsaffinitäten zeigte eine eins zu eins Bindung von PAA mit HSA, die entropisch getrieben ist und strukturellen Untersuchungen weisen eine stabile Proteilstruktur unabhängig von der Adsorption durch PAA auf.
Im zweiten Teil der Arbeit wird die Wechselwirkung zweier uremischer Toxinen, nämlich Phenylessigsäure (PhAA) und Indoxylsulfat (IDS), mit HSA untersucht. Eine wichtige Schlussfolgerung aus der Analyse der ITC Daten ist, dass begünstigende, hydrophobe Wechselwirkungen die treibende Kraft für die Adsorption von Toxinen an HSA sind, und dass hierbei die Enthalpie-Entropie-Kompensation (EEC) zu tragen kommt. Weiterhin zeigen SANS Untersuchungen, dass die Proteinstruktur trotz Adsorption stabil bleibt und konnte außerdem über Interpartikulare Wechselwirkung von HSA-Toxin Komplexen aufklären.
Im Allgemeinen ist HSA strukturell unverändert durch die Adsorption von Liganden. Diese Feststellung erlaubt die Interpretation von ITC Daten, da damit gemessene Wärmeprozesse ausschließlich von Bindungsprozessen herrühren. Die vorliegende Arbeit konnte zeigen, dass eine ausführliche thermodynamische Analyse durch Kombination von theoretischer mit experimenteller Arbeit, eine umfassende Einsicht in die Mechanismen von Bindungsprozessen ermöglicht. / The first part of the thesis explores the charge-charge interaction between proteins and polyelectrolytes. Polyacrylic acid (PAA) is used as a short model polyelectrolyte to interact with human serum albumin (HSA) the most abundand protein in blood, in a comprehensive experimental and theoretical study. The results thereby coincide very well. Computer simulation studies were performed by Xiao Xu within the framework of his PhD thesis. Thermodynamic data were collected by means of isothermal titration calorimetry (ITC) and structural analysis performed using small-angle neutron scattering (SANS). The analysis of binding free energies revealed one to one binding that is mainly driven by entropy. Structural investigations give proof of the stability of the protein beside adsorption.
In the second part, the interaction of two uremic toxins, namely phenylacetic acid (PhAA) and indoxyl sulfate (IDS), with HSA is studied. Systematic ITC experiments reveal two binding sites for both of the two toxins and show small dependence of binding affinities on ionic strength in contrast to PAA adsorption to HSA. This leads to the key conclusion that the favorable hydrophobic interaction is the driving contribution for adsorption and enthalpy-entropy compensation (EEC) effect comes into play. SANS studies of high concentrated HSA-toxin solutions proofed the stability of the protein structure and shed light on the interparticle interaction of HSA-toxin complexes.
In general, HSA is structurally robust regardless of ligand uptake. This finding allows the interpretation of ITC data by confirming that the measured heat signals are purely associated to the binding process. The present thesis has demonstrated that a full thermodynamic analysis in combination with theoretical modelling can provide a comprehensive understanding of binding in terms of identifying driving forces and their contributions to protein ligand interaction.
|
638 |
Korelacija između sastava i svojstava amorfnog As2S3 dopiranog bizmutom / Correlation Between Composition and Properties of Amorphous Bismuth-doped As2S3Šiljegović Mirjana 04 March 2016 (has links)
<p>U ovom radu prikazani su rezultati ispitivanja termičkih, mehaničkih, električnih i optičkih karakteristika kvazibinarnih halkogenida iz sistema Bi-As2S3. Na osnovu termičkih merenja analizirana je kinetika kristalizacionih i predkristalizacionih procesa i utvrđen je mehanizam dekompozicije za različite sastave dobijenih stakala. Primenom impedansne spektroskopije kvantitativno su ocenjeni doprinosi relaksacionih procesa na pojedinim temperaturama u ukupnoj polaraziciji za stakla sa 5 i 7 at.% Bi. Na osnovu merenja Raman spektroskopije identifikovane su nastale strukturne jedinice i konstatovana pojava nanofazne separacije u staklima sa 1.5 i 3 at.% Bi. Mehanička merenja ispitivanih halkogenida različitog sastava ukazala su na povećanje Vickers-ove tvrdoće sa povećanjem udela primesnih atoma. Na osnovu procenjene vrednosti modula elastičnosti ustanovljeno je da uzorak sa 5 at.% Bi odlikuje najgušće atomsko pakovanje. Merenja električnih karakteristika u jednosmernom režimu (DC) pokazala su da je udeo lokalizovanih stanja u ukupnom mehanizmu provođenja značajan samo za manje koncentracije primesnih atoma, a da za veće koncentracije dominantan faktor postaju preskoci između delokalizovanih stanja. Skok u provodljivosti za nekoliko redova veličine kod sastava sa složenijom strukturom protumačen je kao posledica fazne separacije. Rezultati ACmerenja dobijeni za sastav sa 5 at.% Bi ukazali su da je u mernom frekventnom intervalu i dalje dominantan mehanizam termičke aktivacije nosilaca naelektrisanja. Kod sastava sa maksimalnim sadržajem Bi uočena je promena provodljivosti u funkciji frekvencije na svim temperaturama, a dobijeni rezultati su u skladu sa postavkama modela korelisanih preskoka barijere (CHB model).</p> / <p>This paper presents the results of investigation ofthermal, mechanical, electrical and optical propertiesof quasibinar chalcogenides from the system Bi-As2S3. Kinetics analysis of softening and crystallizationprocesses was done on the basis of thermalmeasurements, as well the analysis of decompositionmechanism for different compositions of obtainedglasses. The application of impedance spectroscopy enabled quantitative description of relaxation process contributions at selected temperatures in the overallpolarization for the samples with 5 and 7 at.% Bi. Based on measurements of Raman spectroscopy identification of structural units in the investigated chalcogenides was made, as well as the appearance of nano-scale phase separation in the glasses with 1.5 and 3 at.% Bi. Mechanical measurements pointed to the increase of the Vickers hardness with increase of doping atoms content. Based on the estimated value of the modulus of elasticity it was found that the sample with 5 at.% Bi is characterized by the densest atomic arrangement. Measurements of the electrical properties in dc regime (DC) pointed out that the share of localized states in the whole mechanism of conduction is significant only for the smaller concentrations of doping atoms. For the samples with higher concentrations dominant factor in conductivity are transitions between delocalized states. The jump in conductivity by few orders of magnitude, noticed for the compound with heterogeneous structure was interpreted as a consequence of micro-scale phase separation. Results of ACmeasurements for the composition with 5 at.% Bi showed that the mechanism of thermal activation of charge carriers is still dominant in the measured frequency range. For the composition with the maximum content of Bi changes in conductivity versus frequency were observed at all temperatures, and the results were interpreted in accordance with the model of correlated hopping over the barrier (CHB).</p>
|
639 |
Komparace jednotlivých metod určování bazálního metabolismu / Comparison of methods of basal metabolism determinationKosková, Martina January 2018 (has links)
Title: Comparison of individual methods of basal metabolism determination Objectives: The aim of the work is to compare the individual methods of basal metabolism. These values were measured by indirect calorimetry, plethysmography, bioelectric impedance and predictive equations. Methods: The research was attended by 31 people, including eight men and twenty-three women. All participants of my research were aged 21-30 years. None of the participants was a professional athlete, they were all healthy and none of the women were pregnant or had menstruation. The indirect calorimetry, bioelectronics impedance device Tanita MC - 980 and BOD POD were used to collect the data. Basal metabolic rates were calculated from the prediction equations by Harris & Benedict, Fleisch's equation and Schofield's equation using measured anthropometric values. Results: The results of the methods that have been used for this group of people vary, but the difference is not significant. If we choose as a reference method indirect calorimetry, we can't replace it by any other method. The results for other methods are not significantly different, so we can replace one method with another, except indirect calorimetry. From calculations, we also found out that fat free mass greatly influences the results of basal metabolic rate...
|
640 |
Precipitační procesy v lehkých vytvrditelných slitinách a možnosti začlenění termické analýzy do středoškolské výuky fyziky / Precipitation processes in light hardenable alloys and the possibilities for integrating thermal analysis into physics education on high schoolKodetová, Veronika January 2020 (has links)
The doctoral thesis is divided into two parts - Thermal analysis in physics education on high school and Material research of Al-Zn-Mg(-Cu-Sc-Zr) alloys. Within the first part, the areas of crystallization and/or melting of selected foods were determined using differential scanning calorimetry. A practical lesson for high school physics has been created and tested. The study text focused mainly on differential scanning calorimetry and its use was made. In the second part of the doctoral thesis, there was analysed thermal evolution of the phase transformation in the Al- Zn-Mg(-Cu) alloys with Sc and Zr addition. The effect of (cold and hot) deformation on the decomposition sequences was studied. The hardening effect after annealing above 300 řC in the Sc and Zr alloys is caused by the precipitation of the secondary Al3Sc,Zr) particles. These particles were observed by transmission electron microscopy after annealing up to 360 řC in all studied AlZnMg(Cu)ScZr alloys. In the AlZnMgCu alloy the partial recrystallization was observed after annealing at 350 řC/10 hours and after annealing at 450 řC/10 hours the grain size was 50-200 m (depending on the treatment of the alloy). The addition of Sc, Zr in the AlZnMgCuScZr stabilizes grains and there is no recrystallization in the AlZnMgCuScZr alloy at temperature...
|
Page generated in 0.0637 seconds