Dissertations / Theses on the topic 'Differential scanning calorimetry'
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Thompson, M. "Matrix effects in differential scanning calorimetry." Thesis, Open University, 1991. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.281223.
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Nikolopoulos, Christos. "Mathematical modelling of modulated-temperature differential scanning calorimetry." Thesis, Heriot-Watt University, 1997. http://hdl.handle.net/10399/659.
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Dumitrescu, Oana Roxana. "Simultaneous differential scanning calorimetry : Fourier Transform infrared spectroscopy." Thesis, Cranfield University, 2003. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.421231.
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Jiang, Zhong. "Temperature modulated differential scanning calorimetry : modelling and applications." Thesis, University of Aberdeen, 2000. http://digitool.abdn.ac.uk/R?func=search-advanced-go&find_code1=WSN&request1=AAIU603190.
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The research described in this thesis focused on the TMDSC technique with respect to both theoretical problems and applications. Theoretically, modelling work has been performed to address the effects of heat transfer in the measuring cell on both dynamic and quasi-isothermal TMDSC experiments. The problems of heat transfer generally influence the measured complex heat capacity and phase angle values, but eventually affect the precise measurements of other frequency dependent quantities such as the in-phase and out-of-phase heat capacities. A procedure has been suggested to correct the measured phase angle obtained by dynamic TMDSC using the scaled complex heat capacity trace (Chapter 3). The modulation frequency dependence of the instrumental phase angle has been fully investigated using more realistic models in terms of various heat transfer interface qualities, sample properties and sensor properties. In these models, it is emphasised that the measured temperatures are the sensor temperatures rather than the sample temperatures, thus, the contributions of the sensor's properties to the heat transfer are, for the first time, separated from the overall effects (Chapter 4 and Chapter 5). The consequent effects of heat transfer on the sample's heat capacity measurements are investigated based on the models suggested (Chapter 6). All the modelling results are compared with the corresponding experimental data obtained by ADSC (Mettler-Toledo Ltd) and they are in good agreement. Ripples and fluctuations which appear on the experimental signals during the glass transition and cold crystallisation transition have been simulated using* a simple model in which the period of the modulation signals changes with the time during the transitions, and then, been shown to be artefacts of the Fourier transformation process used by TMDSC evaluations (Chapter 7). The applications of TMDSC to both research and commercial samples are reported in terms of differing either the experimental conditions or the thermal history of the sample. Separating of time dependent kinetic processes from the time independent dynamic processes has been applied on the studies of the glass transition (for polycarbonate and poly(ethylene terephthalate)), the cold crystallisation (for poly(ethylene terephthalate)), the melting transition (for poly(ethylene terephthalate) and lead/tin alloys), the clearing transition of a liquid crystal polymer, and the vitrification of an epoxy resin under quasi-isothermal conditions. The main conclusion drawn from these studies is that the in-phase heat capacity is greatly influenced by the frequency of the temperature modulations even when the underlying heating (or cooling) rate remains the same. This strongly implies that the sample undergoes different structural change under different modulation conditions for the melting transition and clearing transition, but not for the glass transition and cold crystallisation. However, the interpretations of the in-phase heat capacity and out-of- phase heat capacity still need to be clarified. The detection of the glass transition and clearing point for the liquid crystal polymers, and the determination of wax appearance temperature for crude oils, show the ability of TMDSC for combining the sensitivity of a measurement at high instantaneous heating or cooling rates with the resolution obtained by measuring at a low underlying heating or cooling rates. The work on the isothermal curing of the epoxy resins displays the ability of TMDSC on measuring the heat capacity of the sample and its variation under the quasi-isothermal conditions. The frequency dependent complex heat capacity during the glass transition provides a window to measure the apparent activation energy of the transition, which is different, in some extent, from the window used by conventional DSC. The results are correlated by a shift factor. Some shortcomings of TMDSC, however, have been noticed in both modelling and application work. Firstly, any experiments for the purpose of either understanding or the quantitative measurements of TMDSC output quantities should be performed under carefully selected conditions which can satisfy the linear response assumption. Secondly, some signals in particular those associated with kinetic processes may not be fully sampled by TMDSC due to the limit of the observing window of a modulation. Thirdly, when the sensitivity is improved on TMDSC by separating the kinetics processes and noises from the dynamic processes, the TMDSC evaluation procedure introduces mathematical artefacts into the output signals. As a consequence, it is preferable to include as many temperature modulations as possible within any transition being studied in order to obtain good quality experimental signals by eliminating or minimising these artefacts, which, however, is not an easy task for some very abrupt transitions such as melting of metals.
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Murray, John. "A differential scanning calorimetry study of some metal 2,4 pentanedionates." Thesis, Federation University Australia, 1987. http://researchonline.federation.edu.au/vital/access/HandleResolver/1959.17/97253.
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The sublimation enthalpy of beryllium (II), aluminium (III), chromium (III), iron (III), cobalt (III), nickel (II), copper (II), oxovanadium (IV) and zirconium (IV) 2,4 -pentanedionate complexes has been determined by vacuum Differential Scanning Calorimetry (DSC), subsequent to benzoic acid being proposed as calibrant for this technique. In conjunction with existing thermochemical data for these complexes, metal-ligand homolytic bond dissociation energies are calculated and are rationalized in terms of the ionic size of the coordinated meta and the crystal field stabilization energies for the complex. Old and new methods for the determination of sublimation enthalpy are reviewed and the present data collectively reveal the versatility and precision of DSC fort the direct determination of sublimation enthalpies of metal complexes. The new sublimation enthalpy data presented for metal 2-4- pentanedionate complexes effectively ends the controversy associated with the previously reported corresponding data/Master of Applied Science
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Pinto, Rafaela Rocha 1985. "Determinação da capacidade calorífica a pressão constante de ácidos graxos através da calorimetria exploratória diferencial." [s.n.], 2011. http://repositorio.unicamp.br/jspui/handle/REPOSIP/266859.
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Orientador: Maria Alvina KrähenbühlDissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Química
Made available in DSpace on 2018-08-18T13:18:26Z (GMT). No. of bitstreams: 1 Pinto_RafaelaRocha_M.pdf: 1796419 bytes, checksum: 6a9da7357c387302b7688841d36db606 (MD5) Previous issue date: 2011
Resumo: Nos últimos anos tem aumentado o interesse em combustíveis oriundos de fontes renováveis como é o caso do biodiesel. Tendo em vista que os ácidos graxos são componentes de óleos e gorduras, usados para a produção do biodiesel em reações de transesterificação, e cujas propriedades ainda são bastante escassas na literatura, o objetivo do presente trabalho foi o de contribuir com dados experimentais de capacidade calorífica (cp) de ácidos graxos, constituintes de óleos e gorduras. Tais dados são necessários para os balanços de energia e para o projeto de equipamentos visando a purificação de óleos, bem como para o cálculo de reações químicas. A análise térmica diferencial é uma técnica dinâmica que vem sendo muito utilizada na determinação de dados térmicos, como capacidade calorífica, temperaturas de mudanças de estado, determinação da pureza de substâncias, entre outras. O cp é a medida da quantidade de energia necessária por unidade de massa (ou mol) de uma substância para elevar sua temperatura em um grau. Neste trabalho foram determinados os dados de cp dos seguintes ácidos graxos em fase líquida e pressão ambiente: ácido caprílico (C8:0), ácido cáprico (C10:0), ácido láurico (C12:0), ácido mirístico (C14:0), ácido palmítico (C16:0), ácido esteárico (C18:0), ácido oléico (C18:1) e ácido linoléico (C18:2). Para determinar a capacidade calorífica dos ácidos graxos, foi utilizado o Calorímetro Exploratório Diferencial - DSC da TA Instruments. Os dados experimentais foram processados pelo método do software Thermal Specialty Library versão 2.2 e pelo método da Amplitude. Os resultados mostraram que a capacidade calorífica aumenta com a temperatura e com o tamanho da cadeia carbônica. Entre os métodos avaliados não houve diferença entre os resultados obtidos. Os dados experimentais foram comparados com dados obtidos pelo método de contribuição de grupos e os desvios relativos chegaram a 15 %. O intervalo de temperatura de exploração foi de 308 K (35 ºC) a 573 K (300 ºC)
Abstract: In recent years the interest in renewable sources of fuels such as biodiesel has been increasing. Considering that fatty acids are components of fats and oils, used in the production of biodiesel in the transesterification reactions, and whose properties are still quite scarce in the literature, the purpose of this study was to contribute with experimental data of heat capacity (cp) of fatty acid constituents of oils and fats. Such data are needed for energy balances, for the design of equipment aimed at purification of oils and also for the calculation of chemical reactions. Differential thermal analysis is a dynamic technique that has been widely used in the determination of thermal data such as heat capacity, purity determination, phase change temperatures and others. The cp is the amount of energy required per unit mass (or mole) of a substance to raise its temperature by one degree. The cp were determined, in liquid phase and at atmospheric pressure, of the following fatty acids: caprylic acid (C8:0), capric acid (C10:0), lauric acid (C12:0), myristic acid (C14:0), palmitic acid (C16:0), stearic acid (C18:0), oleic acid (C18:1) and linoleic acid (C18:2). To determine the heat capacities of the fatty acids, a Differential Scanning Calorimeter - DSC, of TA Instruments, was used. The experimental data were processed using the Thermal Specialty Library (version 2.2) software and the method of vertical displacement. The results showed that the heat capacity increased with temperature and with the length of the alkyl chains. A comparison of the two methods showed no difference between the resulting information, and when the data from the experiments were compared with the data obtained from the group contribution method, there was a relative deviation of 15%. The working temperature range was from 308 K (35 ºC) to 573 K (300 ºC)
Mestrado
Desenvolvimento de Processos Químicos
Mestre em Engenharia Química
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Gouni, Sreeja Reddy. "Cure Kinetics of Benzoxazine/Cycloaliphatic Epoxy Resin by Differential Scanning Calorimetry." Thesis, California State University, Long Beach, 2018. http://pqdtopen.proquest.com/#viewpdf?dispub=10689461.
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Understanding the curing kinetics of a thermoset resin has a significant importance in developing and optimizing curing cycles in various industrial manufacturing processes. This can assist in improving the quality of final product and minimizing the manufacturing-associated costs. One approach towards developing such an understanding is to formulate kinetic models that can be used to optimize curing time and temperature to reach a full cure state or to determine time to apply pressure in an autoclave process. Various phenomenological reaction models have been used in the literature to successfully predict the kinetic behavior of a thermoset system. The current research work was designed to investigate the cure kinetics of Bisphenol-A based Benzoxazine (BZ-a) and Cycloaliphatic epoxy resin (CER) system under isothermal and nonisothermal conditions by Differential Scanning Calorimetry (DSC). The cure characteristics of BZ-a/CER copolymer systems with 75/25 wt% and 50/50 wt% have been studied and compared to that of pure benzoxazine under nonisothermal conditions. The DSC thermograms exhibited by these BZ-a/CER copolymer systems showed a single exothermic peak, indicating that the reactions between benzoxazine-benzoxazine monomers and benzoxazine-cycloaliphatic epoxy resin were interactive and occurred simultaneously. The Kissinger method and isoconversional methods including Ozawa-Flynn-Wall and Freidman were employed to obtain the activation energy values and determine the nature of the reaction. The cure behavior and the kinetic parameters were determined by adopting a single step autocatalytic model based on Kamal and Sourour phenomenological reaction model. The model was found to suitably describe the cure kinetics of copolymer system prior to the diffusion-control reaction. Analyzing and understanding the thermoset resin system under isothermal conditions is also important since it is the most common practice in the industry. The BZ-a/CER copolymer system with 75/25 wt% ratio which exhibited high glass transition temperature compared to polybenzoxazine was investigated under isothermal conditions. The copolymer system exhibited the maximum reaction rate at an intermediate degree of cure (20 to 40%), indicating that the reaction was autocatalytic. Similar to the nonisothermal cure kinetics, Kamal and Sourour phenomenological reaction model was adopted to determine the kinetic behavior of the system. The theoretical values based on the developed model showed a deviation from the obtained experimental values, which indicated the change in kinetics from a reaction-controlled mechanism to a diffusion-controlled mechanism with increasing reaction conversion. To substantiate the hypothesis, Fournier et al?s diffusion factor was introduced into the model, resulting in an agreement between the theoretical and experimental values. The changes in cross-linking density and the glass transition temperature (Tg) with increasing epoxy concentration were investigated under Dynamic Mechanical Analyzer (DMA). The BZ-a/CER copolymer system with the epoxy content of less than 40 wt% exhibited the greatest Tg and cross-linking density compared to benzoxazine homopolymer and other ratios.
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Snell, Andrew John Roger. "Application of Differential Scanning Calorimetry to Characterize Thin Film Deposition Processes." Cleveland State University / OhioLINK, 2010. http://rave.ohiolink.edu/etdc/view?acc_num=csu1280943337.
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Song, Mo. "Applications of modulated-temperature differential scanning calorimetry to multi-component polymer materials." Thesis, Lancaster University, 1996. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.337256.
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Belkharchouche, Mohamed. "Pressure differential scanning calorimetry studies and its relevance to in-situ combustion." Thesis, University of Salford, 1990. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.280747.
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Martin, A. C. S. "Comb shaped polymer-salt systems : A.C. conductivity and differential scanning calorimetry studies." Thesis, University of Stirling, 1988. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.382751.
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Kuntz, Michael. "Quantifying Isothermal Solidification Kinetics during Transient Liquid Phase Bonding using Differential Scanning Calorimetry." Thesis, University of Waterloo, 2006. http://hdl.handle.net/10012/890.
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The problem of inaccurate measurement techniques for quantifying isothermal solidification kinetics during transient liquid phase (TLP) bonding in binary and ternary systems; and resulting uncertainty in the accuracy of analytical and numerical models has been addressed by the development of a new technique using differential scanning calorimetry (DSC). This has enabled characterization of the process kinetics in binary and ternary solid/liquid diffusion couples resulting in advancement of the fundamental theoretical understanding of the mechanics of isothermal solidification. The progress of isothermal solidification was determined by measuring the fraction of liquid remaining after an isothermal hold period of varying length. A 'TLP half sample', or a solid/liquid diffusion couple was setup in the sample crucible of a DSC enabling measurement of the heat flow relative to a reference crucible containing a mass of base metal. A comparison of the endotherm from melting of an interlayer with the exotherm from solidification of the residual liquid gives the fraction of liquid remaining. The Ag-Cu and Ag-Au-Cu systems were employed in this study. Metallurgical techniques were used to compliment the DSC results. The effects of sample geometry on the DSC trace have been characterized. The initial interlayer composition, the heating rate, the reference crucible contents, and the base metal coating must be considered in development of the experimental parameters. Furthermore, the effects of heat conduction into the base metal, baseline shift across the initial melting endotherm, and the exclusion of primary solidification upon cooling combine to systematically reduce the measured fraction of liquid remaining. These effects have been quantified using a modified temperature program, and corrected using a universal factor. A comparison of the experimental results with the predictions of various analytical solutions for isothermal solidification reveals that the moving interface solution can accurately predict the interface kinetics given accurate diffusion data. The DSC method has been used to quantify the process kinetics of isothermal solidification in a ternary alloy system, with results compared to a finite difference model for interface motion. The DSC results show a linear relationship between the interface position and the square root of the isothermal hold time. While the numerical simulations do not agree well with the experimental interface kinetics due to a lack of accurate thermodynamic data, the model does help develop an understanding of the isothermal solidification mechanics. Compositional shift at the solid/liquid interface has been measured experimentally and compared with predictions. The results show that the direction of tie-line shift can be predicted using numerical techniques. Furthermore, tie-line shift has been observed in the DSC results. This study has shown that DSC is an accurate and valuable tool in the development of parameters for processes employing isothermal solidification, such as TLP bonding.
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Goodman, M. "Differential scanning calorimetry and permeation studies of penetration enhancer and human skin interactions." Thesis, University of Bradford, 1986. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.374906.
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Hill, Vivienne Lucy. "An investigation into the use of MTDSC as a technique for the characterisation of pharmaceutical materials." Thesis, University College London (University of London), 1999. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.322735.
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Hirachand, Katan. "The formation, decomposition and inhibition of clathrate hydrate systems measured by differential scanning calorimetry." Thesis, King's College London (University of London), 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.324673.
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Lee, Jaesung. "Calorimetric and microbiological evaluation of bacteria after exposure to food preservation treatments." Connect to this title online, 2004. http://rave.ohiolink.edu/etdc/view?acc%5Fnum=osu1078597088.
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Thesis (Ph. D.)--Ohio State University, 2004.Title from first page of PDF file. Document formatted into pages; contains xvi, 231 p.; also includes graphics (some col.) Includes bibliographical references (p. 212-224). Available online via OhioLINK's ETD Center
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Bunyaraksh, S. S. "Relation between dyeability of polyester yarn and its structure : Studied by density measurements and differential scanning calorimetry." Thesis, University of Leeds, 1987. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.379540.
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Kirby, Erin. "Study of low temperature nondenaturational conformational change of bovine alpha-chymotrypsin by slow- scanrate differential scanning calorimetry." Thesis, Texas Woman's University, 2014. http://pqdtopen.proquest.com/#viewpdf?dispub=1550669.
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Slow-scan-rate differential scanning calorimetry of enzymes can detect conformational changes which are under kinetic control and not observable at standard scan rates. This method detected a nondenaturational conformational change of bovine &agr;-chymotrypsin at 286 K. This temperature occurs between bovine physiological temperature of 312 K and x-ray crystallography temperature, typically 277 K. This suggests that there are two conformers of &agr;-chymotrypsin, a low temperature conformation and a physiological temperature conformation. The low-temperature to physiological-temperature conformational change has a high activation energy and thus is temperature dependent. The equilibrium thermodynamic changes suggest a reordering of the enzyme structure to give more favorable inter-residue interactions accompanied by an ordering of the structure but one in which there is no change in associated water molecules. The transition state thermodynamics suggest a very strained transition state but one where, again, no change in water interactions is detectable.
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Fischer, Sabine. "Charakterisierung von exothermen Zersetzungsreaktionen mit thermoanalytischen und numerischen Methoden." Tönning Lübeck Marburg Der Andere Verl, 2008. http://d-nb.info/988248646/04.
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Holeman, Teryn A., and Teryn A. Holeman. "Effects of Three Cardiomyopathic-Causing Mutations (D230N, D84N, and E62Q) on the Structure and Flexibility of α-Tropomyosin." Thesis, The University of Arizona, 2017. http://hdl.handle.net/10150/624101.
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Cardiac contraction at the level of the sarcomere is regulated by the thin filament (TF) composed of actin, alpha tropomyosin (TPM), and the troponin (Tn) complex (cTnT: cTnC: cTnI). The "gate-keeper" protein, α-TPM, is a highly conserved α-helical, coiled-coil dimer that spans actin and regulates myosin-actin interactions. The N-terminus of one α-TPM dimer inter-digitates with the C-terminus of the adjacent dimer in a head-to-tail fashion forming the flexible and cooperative TPM-overlap that is necessary for myofilament activation. Two dilated cardiomyopathy (DCM) causing mutations in TPM (D84N and D230N) and one hypertrophic cardiomyopathy (HCM) causing mutation (E62Q), all identified in large, unrelated, multigenerational families, were utilized to study how primary alterations in protein structure cause functional deficits. We hypothesize that structural changes from a single point mutation propagate along the -helical coiled-coil of TPM, thus affecting its regulatory function. Structural effects of the mutations studied via differential scanning calorimetry (DSC) on TPM alone revealed significant changes in the thermal unfolding temperatures of both the C- and N-termini for all mutants compared to WT, indicating that mutational effects propagate to both ends of TPM, thus affecting the overlap region. Although, of note, the proximal termini to the mutation has shown more significant structural changes compared to WT. DSC analysis on fully reconstituted TF’s (Tn:TPM:Actin) revealed effects on the TPM-Actin cooperativity of activation, affecting interaction strength (thermal stability), and the rigidity of TPM moving along actin (FWHM). To characterize the resultant functional effect of these discrete changes in thermal stability and TPM rigidity, ATPase assays were used to measure actomyosin activation in the presence and absence of Ca2+. Together, these data will provide a molecular level understanding of the structural and functional deficits caused by these mutations to help elucidate the mechanisms leading to disease.
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Benedek, Christina. "Synthese und Eigenschaften neuartiger, nichtkristallisierbarer Amphiphile als Baustein für biologische Modellmembranen." [S.l. : s.n.], 2000. http://www.bsz-bw.de/cgi-bin/xvms.cgi?SWB8590236.
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Zander, Patrik, and Johan Hammarström. "Värmebehandling av segjärn med hög kiselhalt." Thesis, Tekniska Högskolan, Högskolan i Jönköping, JTH, Maskinteknik, 2011. http://urn.kb.se/resolve?urn=urn:nbn:se:hj:diva-16377.
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Bakgrunden till detta examensarbete var att Qumex Materialteknik vid ett flertal tillfällen konstaterat att material av typen SS 0725 har uppvisat bristfälliga härdresultat. Materialet, som är relativt nytt på marknaden, är ett gjutjärn av typen segjärn och utmärker sig gentemot andra segjärn på grund av sitt höga innehåll av kisel. Då segjärn enligt den nu gällande EN-standarden klassificeras efter sina mekaniska egenskaper uppstår ett problem gällande SS 0725. Materialet uppfyller de krav som är ställda för EN-GJS-500-7 och hamnar därmed under samma materialbeteckning som ett segjärn med betydligt lägre kiselhalt. Att två material med olika kemisk sammansättning hamnar under samma beteckning kan innebära problem. Syftet med denna rapport är att fastslå vilken påverkan den höga kiselhalten har på materialet vid värmebehandling av typen släckhärdning med efterföljande anlöpning. I försöken ingick fyra material. Det som skiljde materialen åt var halterna av koppar och kisel. De härdades vid tre olika temperaturer och under tre olika tider för att sedan släckas i olja. Målet med släckhärdningen var att materialen skulle få en helt martensitisk struktur vilket då klassades som ett bra härdresultat. Resultatet utvärderades sedan genom optisk mikroskopi och hårdhetsmätningar. En undersökning av materialens fasomvandlingstemperaturer genomfördes med hjälp av Differential Scanning Calorimetry. Resultatet visar att kiselhalten har stor påverkan på den temperatur som krävs för att erhålla ett bra härdresultat. För material med låg kiselhalt uppnåddes fullständig martensitbildning efter släckhärdning från 840°C. För material med hög kiselhalt uppnåddes liknande strukturella och hårdhetsmässiga resultat först vid en så hög temperatur som 900°C och behandlingstider längre än 1 h. Den relativa skillnad som uppmättes i fasomvandlingstemperatur med hjälp av Differential Scanning Calorimetry mellan högkiselmaterial och lågkiselmaterial var 45°C. Detta resultat kombinerat med analyserna av härdprocesserna visar att det krävs kraftigt ökad temperatur vid värmebehandling av högkiselmaterialet SS 0725.The background to this thesis was that Qumex Materialteknik at several occasions had received material of type SS 0725 that had shown deficient heat treatment results. The material, which is relatively new, is a cast iron of type ductile iron and differ against other ductile irons because of its high silicon content. According to EN standard ductile irons are classified by their mechanical properties. A problem then occurs with the new material SS 0725 because of this. The material fulfils the requirements for EN-GJS-500-7 and is therefore in the same classification as a ductile iron with much lower silicon content. Two materials having major differences in chemical composition ending up in the same classification can be problematic. The purpose of this report is to determine impact of high silicon content in ductile iron when heat treated and quench hardened. The experiment included four materials, and the major difference between the materials were their content of copper and silicon. The heat treatment process was performed at three different temperatures and three different treatment times. Afterwards the samples were quenched in oil. The ambition of the quench hardening was to obtain a material structure of 100% martensite. By optical microscopy and hardness measurements the results then were evaluated. An investigation of the phase transformation temperature in the materials was made by using Differential Scanning Calorimetry. The results show that the amount of silicon content has great influence on the temperature for receiving good hardening results. To achieve 100% martensite after quench hardening in materials with low silicon content the temperature needs to be over 840°C. For material with high level of silicon content the temperature for achieving 100% martensite needs to be 900°C and the treatment time should be over 1 h. The relative difference in phase transformation temperature was measured using Differential Scanning Calorimetry. The results of the measurements between the materials with high silicon content and materials with low silicon content was 45°C. This result combined with the analysis of the heat treatment process shows that a major increase of the temperature is needed to heat treat SS 0725.
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Hoyle, N. D. "The characterisation of the adsorptive and catalytic properties of supported platinum metal catalysts by methods including differential scanning calorimetry." Thesis, Brunel University, 1985. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.370135.
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Pöhlmann, Milena. "Thermisch härtende Polymerverbundmaterialien als Basis für neue Befestigungssysteme." Doctoral thesis, Saechsische Landesbibliothek- Staats- und Universitaetsbibliothek Dresden, 2006. http://nbn-resolving.de/urn:nbn:de:swb:14-1165492370619-99312.
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Mit der Entwicklung und Einführung ökologischer Bauweise im Neubau sowie neuen Baustoffsystemen in Sandwichbauweise wird es zunehmend erforderlich, neue effektive Befestigungsvarianten zu entwickeln, die eine dauerhafte Fixierung auch unter sicherheitstechnischen Bestimmungen sowie aus Garantie- bzw. haftungsrechtlichen Gründen ermöglichen. Die aus der Praxis bisher bekannten chemischen Befestigungssysteme (Zweikomponentenverbundmörtel, Verbundankerpatronen) weisen hinsichtlich der Applikation unter bautechnischen Bedingungen noch einige Nachteile auf. Dazu gehören vor allem längere Aushärtungszeiten zur Realisierung der abschließenden Verbundfestigkeit, Inhomogenitäten im Verbund, der Einsatz toxischer Verbindungen und eine Limitierung der Applikationsmöglichkeiten in horizontalen und Überkopf-Einsatzbereichen sowie Hohlkammersystemen. Alle zuvor genannten Punkte haben bis jetzt die Nutzung solcher Verbundwerkstoffe als universale Anwendungsmöglichkeit verhindert. Ein neues chemisches Befestigungssystem, welches aus Novolak gehärteten mit Hexamethylentetramin (Hexa) und anorganischen Füllstoff besteht, wurde für Applikationen in Beton entwickelt. Das Bindemittel härtet bei der Temperaturzuführung aus. Die unkatalysierte Befestigungsmasse zeigt bei einer Temperatur zwischen 150-300 °C eine hohe Reaktivität. Die Vorteile dieses Systems sind die unbegrenzte Lagerfähigkeit der vorgemischten härtbaren Masse sowie die Gewährleistung einer homogenen Netzwerkstruktur im gesamten Verbund und sie ist frei von giftigen und flüchtigen Substanzen. Auf den Einsatz toxischer Substanzen wurde verzichtet. In dieser Arbeit wurde die Gesamtkinetik der Reaktion während des Aushärtungsprozesses dieser Polymerkomposite untersucht. Die DSC- (nicht-isothermen, isothermen) und MDSC-Untersuchungen haben sich als ein sicheres Verfahren zur Qualitätskontrolle des Aushärtezustands der Befestigungssysteme herausgestellt. Parallel zur nicht-isothermischen und isothermischen DSC wurden Leitfähigkeitsmessungen durchgeführt, um den Endpunkt der Aushärtungsreaktion zu bestimmenThe development and introduction of ecological construction methods and the use of sandwich materials make it necessary to develop new fixing systems and technologies. Dealing with the application in concrete and other substrates commercial chemical fixing systems show some disadvantages up to date. Especially the rather long curing time in order to realize the final bond strength, inhomogenities in the composite, the partial use of toxic substances and application limits of such systems in horizontal direction as well as hollow section materials has so far prevented the use of such composites for all-purpose applications. A new chemical fixing system, which consists of hexamethylene tetramine (hexa) cured novolac and inorganic filler, was developed for application in concrete. It is applied by a thermo-curing procedure. The uncatalyzed curable mixture has a high reactivity at temperature between 150-300 °C. Compared with commercial chemical fixing systems, the premixed curable mass has many benefits. First it has a unique storage stability and second, it is free of toxic and volatile substances. Another important aspect is, it is self-foaming. In this study was investigated the overall kinetics of the reaction during the curing process of these polymer composites. An appropriate method for this experiment proved to be the DSC in isothermal and non-isothermal mode and MDSC. This turned out to be a safe quality control technique for these systems. Parallel to the non-isothermal and isothermal DSC conductivity measurements have been performed to determine the end point of the curing reaction
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Oliveira, Levi Ezequiel de. "Análise térmica dos biodieseis obtidos por rota enzimática e suas respectivas matérias-primas." Universidade de São Paulo, 2010. http://www.teses.usp.br/teses/disponiveis/97/97136/tde-03102012-121140/.
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A maior parte de toda a energia consumida no mundo provém do petróleo, carvão e gás natural (87% da matriz energética mundial). No entanto, essas fontes não renováveis possuem previsão de esgotamento em um futuro próximo. Além disso, são poluidores, afetando o meio ambiente, motivando a sociedade buscar fontes alternativas para mitigar esses problemas. O biodiesel, como alternativa de combustível, começou a ser estudado em 1937, e hoje mostra ser uma alternativa eficiente e não poluidora à utilização do diesel mineral. O estudo presente foi realizado com amostras de biodieseis obtidos utilizando catalisadores enzimáticos. Essa rota vem sendo investigada no país por diversos pesquisadores, e vem mostrando que o uso da enzima como catalisador minimiza os problemas relativos às etapas finais de purificação do biodiesel, pois reduz a ocorrência das reações indesejáveis de saponificação e permite uma simplificação e redução dos custos dos processos pela diminuição do número de operações associadas. Para ser um substituto, o biodiesel precisa se enquadrar em normas, no caso do Brasil, a resolução nº 42 da ANP (Agência Nacional de Petróleo, Gás Natural e Biocombustíveis) de 2004. Além disso, deve possuir qualidades que viabilize a sua substituição. Esse trabalho tem o objetivo de realizar o estudo térmico utilizando a Termogravimetria (TG) e a Calorimetria Exploratória Diferencial (DSC) dos biodieseis de babaçu, palma e sebo bovino obtidos pela rota enzimática e suas respectivas matérias-primas. Com os resultados da TG em atmosfera Inerte, foi possível analisar a volatilidade desses biodieseis, e também verificar o seu enquadramento no parâmetro de destilação da resolução nº 42 da ANP. A TG em atmosfera oxidativa possibilitou comparar esses biodieseis em relação às suas estabilidades termo-oxidativas. Também foram realizados o Estudo Cinético das curvas TG, visando o valor da energia de ativação das primeiras etapas de cada curva, utilizando o modelo matemático Ozawa. O estudo cinético das curvas TG em atmosfera de nitrogênio mostrou que a energia de ativação e a temperatura de inicio da degradação têm uma relação direta.Most of all energy consumed worldwide comes from oil, coal and natural gas (87% of global energy production). However, these non-renewable resources are expected to exhaust in the near future. Moreover, they are polluters, affecting the environment, prompting the company to seek alternative sources to mitigate these problems. Biodiesel as alternative fuel, that began to be studied in 1937 and today has proved an efficient and non-polluting alternative to the use of mineral diesel. The present study was performed with babassu, palm and tallow biodiesel obtained using enzymatic catalysts. This route has been investigated by several researchers in the country, and has shown that the use of enzyme as catalyst minimizes the problems related to the final stages of purification of biodiesel, it reduces the occurrence of undesirable reactions of saponification and allows for simplification and cost reduction processes by reducing the number of associated operations. To be a substitute, biodiesel must fit in standards, in the case of Brazil, the resolution No. 42 of the ANP (National Agency of Petroleum, Natural Gas and Biofuels), 2004. Also this biofuel must posses qualities thet might allow the replacement. This work aims to realize the thermal studies using thermogravimetry (TG) and Differential Scanning Calorimetry (DSC) of babassu, palm and tallow biodiesel obtained by enzymatic route and also their raw materials. With the results of TG in an inert atmosphere, it was possible to analyze the volatility of biodieseis, and also check your guidelines on the parameter of the distillation of Resolution No. 42 of the Brazilian Petroleum Agency (ANP). The TG analysis of biodiesel in oxidative atmosphere turns possible to study their thermo-oxidative stabilities. Also, it was performed a kinetic study of the TG curves, seeking the value of activation energy of the first steps of each curve, using the mathematical model Ozawa. The kinetic study of the TG curves in nitrogen atmosphere showed that the activation energy and temperature of the beginning of degradation have a direct relationship.
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Chabalenge, Billy, Sachin A. Korde, Adrian L. Kelly, Daniel Neagu, and Anant R. Paradkar. "Understanding Matrix Assisted Continuous Cocrystallisation using Data Mining approach in Quality by Design (QbD)." ACS, 2020. http://hdl.handle.net/10454/18005.
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NoThe present study demonstrates the application of decision tree algorithms to the co-crystallization process. Fifty four (54) batches of carbamazepine–salicylic acid co-crystals embedded in poly(ethylene oxide) were manufactured via hot melt extrusion and characterized by powder X-ray diffraction, differnetial scanning calorimetry, and near-infrared spectroscopy. This dataset was then applied in WEKA, which is an open-sourced machine learning software to study the effect of processing temperature, screw speed, screw configuration, and poly(ethylene oxide) concentration on the percentage of co-crystal conversion. The decision trees obtained provided statistically meaningful and easy-to-interpret rules, demonstrating the potential to use the method to make rational decisions during the development of co-crystallization processes.
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Pisch-Heberle, Sandra. "Untersuchungen zur Stabilisierung von Membranproteinen mit ungewöhnlichen Phospholipiden." [S.l.] : Universität Stuttgart , Fakultät Chemie , Institut für Technische Biochemie, 2000. http://www.bsz-bw.de/cgi-bin/xvms.cgi?SWB8619088.
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Wampler, Amos. "Resolution of crystalline phases in polymorphic gel-spun ultra-high molecular weight polyethylene fibers using restrained differential scanning calorimetry and x-ray diffraction." Access to citation, abstract and download form provided by ProQuest Information and Learning Company; downloadable PDF file, 70 p, 2008. http://proquest.umi.com/pqdweb?did=1597633731&sid=6&Fmt=2&clientId=8331&RQT=309&VName=PQD.
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Kumar, Prateek. "Heat Capacity and Oxidation Kinetic Studies of Fe-Ti Composite Metal Oxide (ITCMO) using Simultaneous Differential Scanning Calorimetry and Thermogravimetric Analysis." The Ohio State University, 2017. http://rave.ohiolink.edu/etdc/view?acc_num=osu1502723527531035.
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Santos, Monique Barreto. "Estudo da forma??o dos complexos coacervados obtidos a partir de prote?nas globulares." Universidade Federal Rural do Rio de Janeiro, 2016. https://tede.ufrrj.br/jspui/handle/jspui/1297.
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Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico - CNPq
Proteins are biopolymers of high nutritional and functional significance has been widely used as food ingredients. The interaction between two different proteins oppositely charged, and can give rise to complex coacervate currently used as an ingredient in food technology or as a microencapsulating agent. The formation of complex coacervates between Lysozyme and Ovalbumin and between Bovine serum albumin (BSA) and Lysozyme has been investigated as a function of pH, mass ratio of total and concentration of NaCl. For both interactions studied, complexing latched in a wide pH range which corresponds to the interval between the pI of proteins. Among Ovalbumin and Lysozyme interaction was more intense in the ratio r = 1 at pH 7.5 and BSA and Lysozyme most complex formation has occurred on the ratio r = 0.5 and pH 9.0. Changes in the ionic strength by adding NaCl negatively affected the interaction between Lysozyme and BSA already at a concentration of 0.01 mol / L and 0.03 mol / L abolished the interaction between Lysozyme and Ovalbumin. Through Potential - zeta can be seen that the formation of insoluble complexes was highest near the pI for all studied reasons, indicating that the interaction is given by neutralization of opposite charges. The Infrared spectra suggested that electrostatic interactions led interactions however, hydrogen bonds also had a hand in the coacervation process for the proteins under study. The micrographs showed that the insoluble complexes showed spherical structure and particle size showed the formation of structures with an average size around 2 ?m, much larger than the observable size for the isolated proteins. The isothermal titration calorimetry showed that the interaction between Lysozyme and Ovalbumin was exothermic and was performed in two steps, the first and second entropy directed enthalpy driven. The differential scanning calorimetry suggested the presence of a single point of denaturation, that the interaction between Lysozyme and BSA led to a new biopolymer with denaturation temperature 67 ? C differs from isolated proteins. These studies suggested that complex coacervates formed between Ovalbumin / Lysozyme and BSA / Lysozyme could be used as the encapsulating bioactive agent or as food ingredients in order to add nutritional value.
Prote?nas s?o biopol?meros de grande import?ncia nutricional e funcional tendo sido amplamente utilizadas como ingredientes alimentares. A intera??o entre duas prote?nas diferentes e opostamente carregadas pode dar origem aos complexo coacervado, atualmente utilizados como ingrediente na tecnologia de alimentos ou como agente de microencapsula??o. A forma??o de complexos coacervados entre Ovalbumina e Lisozima e entre Albumina s?rica bovina (BSA) e Lisozima foi investigada em fun??o do pH, raz?o de massa total e concentra??o de NaCl. Para as duas intera??es estudadas, a complexa??o acorreu em uma ampla faixa de pH, que corresponde ao intervalo entre os pI das prote?nas. Entre Ovalbumina e Lisozima a intera??o foi mais intensa na raz?o r=1 em pH 7,5 e para BSA e Lisozima a maior forma??o de complexos ocorreu na raz?o r=0,5 e pH 9,0. Altera??es na for?a i?nica por adi??o de NaCl influenciaram negativamente a intera??o entre Albumina BSA e Lisozima j? na concentra??o de 0,01 mol/L e a 0,03 mol/L suprimiu a intera??o entre Ovalbumina e Lisozima. Por meio do Potencial - zeta pode-se verificar que a forma??o de complexos insol?veis foi m?xima pr?ximo ao pI para todas as raz?es estudadas, indicando que a intera??o se deu por neutraliza??o de cargas opostas. Os espectros no infravermelho sugeriram que intera??es eletrost?ticas conduziram as intera??es no entanto, liga??es de hidrog?nio tamb?m tiveram participa??o no processo de coacerva??o para as prote?nas em estudo. As micrografias revelaram que os complexos insol?veis apresentavam estrutura esf?rica e o tamanho de part?cula demonstrou a forma??o de estruturas com tamanho m?dio em torno de 2 ?m, as quais s?o bem maiores do que o tamanho obervado para as prote?nas isoladas. A calorimetria de titula??o isot?rmica demonstrou que a intera??o entre Ovalbumina e Lisozima foi exot?rmica, a qual ocorreu em duas etapas, a primeira entropicamente dirigida e a segunda entalpicamente dirigida. A calorimetria diferencial de varredura sugeriu, pela presen?a de um ?nico ponto de desnatura??o, que a intera??o entre BSA e Lisozima deu origem a um novo biopol?mero com temperatura de desnatura??o a 67?C, diferente das prote?nas isoladas. Estes estudos sugeriram que complexos coacervados formados entre Ovalbumina / Lisozima e BSA / Lisozima poderiam ser utilizados como agente encapsulante de bioativos ou como ingredientes alimentares com o objetivo de agregar valor nutricional.
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LINS, Taynara Batista. "Estudo de correlação dos parâmetros térmicos e difração de raios x de diferentes cristais e dispersões sólidas de atorvastatina." Universidade Federal de Pernambuco, 2015. https://repositorio.ufpe.br/handle/123456789/16563.
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CNPq
Este estudo teve como finalidade desenvolver metodologias analíticas para os estudos de caracterização do estado sólido do fármaco atorvastatina cálcica e, também, das suas dispersões sólidas pelas correlação das técnicas difratometria de Raios X (DRX), espectroscopia de infravermelho (FTIR) e analise térmica (DSC e TG). A atorvastatina cálcica (ATC) é um agente redutor de lipídios sintético, que já tem muitos polimorfos relatados na literatura. No estudo de caracterização no estado sólido do fármaco, foram obtidos cristais da ATC com solventes de graus de polaridade diferentes e foi observado que os solventes clorofórmio, etanol e metanol levaram a formação de uma estrutura cristalina mais amorfa, e essa alteração estrutural foi perceptível no FTIR com alteração na banda do estiramento da hidroxila e pelos dados de DSC como diminuição da entalpia e desaparecimento do pico de fusão. Enquanto que, solventes éter e acetato de etila não levaram a mudança no habito cristalino quando comparado com o fármaco antes do processo de recristalização. As dispersões sólidas foram feitas com 5 surfactantes diferentes (carbopol®, hidroxipropil metil celulose (HPMC), lauril sulfato sódio, polietileno glicol (PEG) 6000 e carbopol-ultrez® 20) e pela correlação do dados DRX, FTIR e DSC foi visto que a dispersão com carbopol-utlrez foi a que apresentou grande interação com mudanças nas banda de absorção e desaparecimento do pico de fusão. Ao avaliarmos a estabilidade das dispersões por termogravimetria, observou-se que todas elas tinham menor estabilidade que a ATC. Esses resultados apontam para a utilidade de técnicas de análise térmica como uma ferramenta de triagem relevante para a caracterização do estado sólido durante o desenvolvimento de formulação. Através da análise multivariada foi possível estabelecer a correlação entre a técnicas estudadas mostrando a relevância da utilização destas na avaliação dos parâmetros de controle qualidade de processos e produtos farmacêuticos.
This study aimed to develop analytical methods for the characterization studies of solid state drug atorvastatin calcium and also their solid dispersions by the correlation of techniques: X-ray diffraction (XRD), infrared spectroscopy (FTIR) and thermal analysis (DSC and TG). The atorvastatin calcium (ATC) is a reducing agent synthetic lipids, which already has many polymorphs reported in the literature. In the characterization studies in the solid state of the drug, ATC crystals were obtained with different degrees of polarity solvent and it was observed that the solvents chloroform, ethanol and methanol led to formation of a more amorphous crystal structure, and this structural change was noticeable in FTIR with changes in the band of the hydroxyl stretch and by the DSC data as decreased enthalpy and disappearance of the melting peak. While, ether and ethyl acetate solvents did not lead to change in the crystal habit when compared with the drug before the recrystallization process. Solid dispersions were made with 5 different surfactants (Carbopol®, hydroxypropyl methyl cellulose (HPMC), sodium lauryl sulfate, polyethylene glycol (PEG) 6000 and carbopol-ultrez® 20) and by the correlation data of XRD, FTIR and DSC was seen that the dispersion with carbopol-utlrez showed the great interaction with changes in absorption band and disappearance of the melting peak. In evaluating the stability of the dispersions by thermogravimetric analysis, it was observed that all of them had lower stability than ATC. These results point to the utility of thermal analysis techniques as an important screening tool for the characterization of the solid state during the development of formulation. Through multivariate analysis was possible to establish the correlation between the techniques studied shows the importance of using these in the evaluation of the quality control parameters of process and pharmaceuticals.
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VIANA, Waleska Pereira. "Estudo de caracterização do estado sólido de diferentes cristais e dispersões sólidas do anlodipino." Universidade Federal de Pernambuco, 2015. https://repositorio.ufpe.br/handle/123456789/16571.
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CAPES
O besilato de anlodipino é um antagonista dos canais de cálcio, utilizado como um anti-hipertensivo e anti-isquêmico, sendo utilizado como uma mistura racêmica dos enantiômeros S e R, dos quais o S-anlodipino é o que apresenta maior atividade como bloqueador de cálcio. Por tanto, o objetivo desse estudo foi caracterizar as formas cristalinas do besilato de anlodipino e correlacionar os parâmetros térmicos e analíticos das dispersões sólidas do besilato de anlodipino obtidas por liofilização. Os ângulos vistos no DRX demonstraram a presença de uma estrutura cristalina anidra, para o AMB. Os deslocamentos nos comprimentos de onda no espectro de infravermelho (FTIR) do cristal do AMBACt corroboraram com os resultados do DRX que apresentou mudança no tamanho dos cristalitos, além disso a curva de DSC apresentou dois picos endotérmicos diferentemente do fármaco, com apenas um processo endotérmico e grau de pureza de 96%. A energia cinética de ativação (Ea = 121,6 KJ mol-1 ±1,2), o fator de frequência (A = 27,87 ± 4,1 min-1), e a ordem de reação (n = 0) da etapa principal da decomposição térmica do AMB foram realizadas de acordo com o Modelo de Ozawa. No estudo das dispersões sólidas, os dados do DRX para o AMBHPMC apresentou amorfização e essa alteração no arranjo cristalino também foi evidenciada nos resultados encontrados no FTIR, com deslocamentos nas bandas de intensidade, supressão e aparecimento de novas bandas. Além disso, o método termoanalítico mostrou supressão e deslocamento dos picos de fusões das dispersões sólidas, e perda de massa diferente do fármaco. Portanto, juntas, as técnicas colaboraram para a caracterização das formas cristalinas, e nos estudos de compatibilidade fármaco-excipiente através avaliação das interações físico-químicas nas dispersões sólidas.
The amlodipine besylate is a calcium channel antagonist used as antihypertensive and anti- ischemic , and used as a racemic mixture of R and S enantiomers , of which the S- amlodipine is what is more active as blockers calcium. Therefore, the aim of this study was to characterize the crystalline forms of amlodipine besylate and correlate the thermal and analytical parameters of solid dispersions of amlodipine besylate obtained by lyophilization. The angles viewed XRD showed the presence of an anhydrous crystalline structure for the AMB. The shifts in wavelengths in the infrared spectrum (FTIR) of the AMBACt crystal corroborate with the results of the XRD which showed change in the size of the crystallites, furthermore the DSC curve showed two endothermic peaks unlike the drug with only one process endothermic and purity of 96%. The activation kinetic energy (Ea = 121.6 kJ mol-1 ± 1.2), the frequency factor (A = 27.87 ± 4.1 min-1) and the reaction order (n = 0) of the main stage of AMB thermal decomposition were performed according to the Ozawa model. In the study of of the solid dispersions, the XRD data for AMBHPMC which showed amorphization and this change in the crystalline arrangement was also evidenced in the results found in the FTIR, with shifts in intensity bands, suppression and appearance of new bands. Also, the thermal method proved suppression and displacement of the melting peaks of the solid dispersions and loss of mass different than drug. Porting together the characterization techniques contributed to the evaluation of crystalline forms, and of the physicochemical interactions in solid dispersions.
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Bento, Ronaldo Euzébio. "Estudo do comportamento da resina base na formulação de compósitos de politetrafluoretileno com bronze." [s.n.], 2011. http://repositorio.unicamp.br/jspui/handle/REPOSIP/266830.
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Orientador: João Sinézio de Carvalho CamposDissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Química
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Resumo: Esse trabalho concentra os estudos na investigação das propriedades de resistência a tração e alongamento do compósito de Politetrafluoretileno (PTFE) com 60% de bronze após a substituição do tipo de PTFE utilizado na formulação desse compósito. Atualmente esse compósito utiliza PTFE convencional na formulação e o objetivo é alterar para PTFE modificado. A motivação para essa alteração deveu-se ao fato que o PTFE convencional apresenta disponibilidade limitada dificultando o desenvolvimento dos segmentos que utilizam os compósitos de PTFE com 60% de bronze. A escolha do PTFE modificado para a substituição do PTFE convencional na formulação do compósito de PTFE com 60% de bronze deveu-se ao fato que polímero puro de PTFE modificado apresenta propriedades mecânicas e químicas superiores ao polímero puro de PTFE convencional, além de não apresentar limitações de disponibilidade, possibilitando a continuidade do crescimento dos segmentos industriais. A escolha do compósito de PTFE com 60% de bronze deveu-se ao fato que essa formulação é a mais empregada no segmento automobilístico para a fabricação de anéis para amortecedores e retentores. Após a substituição da resina de PTFE, os resultados demonstraram que o compósito de PTFE modificado com 60% de bronze apresentou propriedades inferiores ao compósito fabricado com PTFE convencional. A queda dessas propriedades pode estar relacionada com possíveis micros fissuras na estrutura do compósito em virtude de ar preso durante o processo de fabricação
Abstract: This work focuses on research studies of the properties of tensile strength and elongation of the composite of Polytetrafluoroethylene (PTFE) with 60% bronze after replacing the type of PTFE used in the formulation of this compound. Currently, this composite uses conventional PTFE in the formulation and the objective is to change to modified PTFE. The motivation for this change was due to the fact that the conventional PTFE has limited availability hindering the development of the segments that use the PTFE composite with 60% bronze. The choice of PTFE modified PTFE to replace the conventional formulation of the composite with 60% PTFE bronze was due to the fact that pure polymer modified PTFE has superior mechanical and chemical properties of the pure polymer PTFE conventional, and not present availability limitations, enabling the continued growth of industries. The choice of the composite with 60% PTFE bronze due to the fact that this formulation is the most used in the automotive sector for the manufacture of rings and seals for shock absorbers
Mestrado
Ciencia e Tecnologia de Materiais
Mestre em Engenharia Química
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Denari, Gabriela Bueno. "Contribuições ao ensino de análise térmica." Universidade de São Paulo, 2013. http://www.teses.usp.br/teses/disponiveis/75/75135/tde-04042013-151955/.
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Considerando a importância crescente das técnicas termoanalíticas na indústria e na pesquisa contemporânea, torna-se necessário apresentá-las de forma adequada aos alunos de cursos de graduação, não apenas de química, mas de ciência dos materiais, física, farmácia, das diversas modalidades de engenharia, entre outros. Por outro lado, pode-se notar que isso raramente acontece, por diversos motivos, como falta de equipamentos, falta de experimentos demonstrativos das técnicas e até mesmo de falta de preparo dos docentes, com relação ao conhecimento dos fundamentos das técnicas e normalização de nomenclatura. No sentido de contribuir com o ensino de Análise Térmica em nosso país, este trabalho teve por objetivo buscar informações históricas e compilar e/ou desenvolver experimentos didáticos que possam ser usados na demonstração de conceitos teóricos e aspectos práticos das técnicas termoanalíticas mais usadas no Brasil, como a Termogravimetria (TGA), Termogravimetria Derivada (DTG), Análise Térmica Diferencial (DTA) e Calorimetria Exploratória Diferencial (DSC). Para avaliar o efeito didático do material desenvolvido foi proposto um curso extracurricular no tema Análise Térmica, chamado \"Princípios e Aplicações de Análise Térmica\", em nível de graduação na forma de curso de Difusão Cultural, apoiado pela Pró-Reitoria de Cultura e Extensão da Universidade de São Paulo (USP). Participaram 12 alunos de graduação e 3 alunos de pós-graduação, estes últimos como ouvintes. Os participantes receberam material didático escrito, na forma de uma apostila, instruções teóricas e aulas práticas, envolvendo experimentos com problemas práticos contextualizados, em Análise Térmica. A avaliação do curso foi feita com base em questionários sobre expectativas dos alunos em relação ao curso, seus conhecimentos prévios e aqueles obtidos ao final do curso. Os questionários foram aplicados antes e após as atividades. A avaliação de conteúdo foi feita usando questões sobre o tópico abordado e revelou significativo ganho de conhecimento desses alunos em relação às técnicas termoanalíticas. Assim, atingiu-se o esperado, contribuindo de alguma maneira para o ensino de Análise Térmica e sua aplicação nos cursos de graduação, envolvendo Termogravimetria, Termogravimetria Derivada, Análise Térmica Diferencial e Calorimetria Exploratória Diferencial.Considering the increasing relevance of the thermoanalytical techniques in both industry and contemporary research, it becomes interesting to present such techniques in a proper way to undergraduate students, not only in chemistry, but also in materials science, physics, pharmacy, the several areas of engineering, and other potential users of these techniques. Moreover it can be noted that this rarely happens due to many reasons such as unavailability of equipments, to demonstrate the experimental details and even lacking in knowledge of professors regarding the fundamentals of the techniques and standardization in nomenclature. In order to contribute to the Thermal Analysis education in Brazil, this study aimed to seek historical information and compilation and/or development of didactic experiments that can be used in the demonstration of theoretical concepts and practical aspects of the most commonly used thermoanalytical techniques, such as Thermogravimetry (TGA), Derivative Thermogravimetry (DTG), Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC). Beyond that, it was necessary to apply these contents with undergraduate volunteer students. Therefore, an extracurricular Thermal Analysis course in this subject, named \"Principles and Applications of Thermal Analysis\", supported by the Dean of Culture of the Universidade de São Paulo (USP) was offered. Twelve undergraduate and three graduate students from four Universities of São Paulo State attended the course. These students received educational written materials in the form of a handout, instructions in theoretical aspects and practical sessions involving experiments, represented by practical problems in Thermal Analysis. The course evaluation was based on questionnaires about students\' expectations and their previous knowledge and that obtained by the end of the activity. The scope evaluation was made using questions about the topics covered and revealed significant improvement in the knowledge of the students regarding the thermoanalytical techniques covered in the course. Thus the expectations of the dissertation have been satisfied in developing a written material for thermal analysis education covering historical aspects as well as, theoretical and practical concepts of Thermogravimetry, Differential Thermal Analysis, Differential Thermal Analysis and Differential Scanning Calorimetry and their application to undergraduate courses.
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Ding, Shu. "Thermodynamic studies on iron-sulfur cluster assembly proteins." The Ohio State University, 2011. http://rave.ohiolink.edu/etdc/view?acc_num=osu1316472363.
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Buyukyagci, Arzu. "Synthesis And Characterization Of Monoacetylferrocene Added Sulfonated Polystyrene Ionomers." Master's thesis, METU, 2004. http://etd.lib.metu.edu.tr/upload/3/1108026/index.pdf.
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Incorporation of monoacetylferrocene to the sulfonated polystyrene
ionomers imparted some changes in the properties of sulfonated polystyrene.
Sulfonation was carried out by acetic anhydride and concentrated sulphuric acid.
The sulfonation reaction and the degree of sulfonation were determined by
analytical titration and adiabatic bomb calorimeter .
For this purpose, sulfonated polystyrene (SPS) samples with varying
percentages of sulfonation were prepared between 0.85% and 6.51%. Monoacetyl
ferrocene was used in equivalent amount of sulfonation through addition
procedure.
FTIR Spectroscopy was one of the major techniques used to support the
successful addition of AcFe to the SPS samples. Altering the sulfonation degree
did not change the characteristic peak positions, but increased the peak intensities
with increasing the degrees of sulfonation.
Mechanical properties of resultant polymers were investigated. As a result,
elastic modulus of polymers decreased by the amount of monoacetylferrocene.
Thermal characteristic were found by Differential Scanning Calorimeter
(DSC). Thermal analysis revealed that sulfonated polystyrene samples after
addition of monoacetylferrocene displayed lower values of Tg.
Microscopic analysis were made by Scanning Electron Microscopy (SEM)
and single phase for each sample was observed. Besides, energy dispersed micro
analysis showed an increase in the intensity of the iron (II) peaks that is related to
the amount of monoacetylferrocene added to the SPS samples.
Flame retardancy for each polymer was also examined and found that
addition of monoacetylferrocene to sulfonated polystyrene does not change the
Limiting Oxygen Index value (LOI)(17). However, LOI value for polystyrene is
18.
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Young, Gregory Scott. "The application of thermal microscopy, differential scanning calorimetry, and fourier transform infrared microspectroscopy to characterize deterioration and physiochemical change in fibrous Type 1 collagen." Thesis, University College London (University of London), 1999. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.420072.
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Almutairi, Badriah Saad. "Correlating Melt Dynamics with Glass Topological Phases in Especially Homogenized Equimolar GexAsxS100-2x Glasses using Raman Scattering, Modulated- Differential Scanning Calorimetry and Volumetric Experiments." University of Cincinnati / OhioLINK, 2020. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1593272974284834.
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Blomdahl, Emil. "Synthesis and characterization of novel hybrid organic-inorganic materials." Thesis, KTH, Tillämpad fysikalisk kemi, 2021. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-302288.
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Efterfrågan på bättre och mer hållbart material ökar. Mer effektivt material kommer att behövas för att möta den ökande, globala efterfrågan. Hybrida organiska-oorganiska material är en typ av material som har varit av stort intresse nyligen, och kan beskrivas som en typ av material som består av både organiska och oorganiska komponenter. Denna avhandling har fokuserat på hybrida organiska-oorganiska material inspirerade av den klassiska perovskitstrukturen ABX3, där komponent A är en organisk katjon, komponent B är en divalent metalkatjon och komponent X är en anjon. Hybrida organiska-oorganiska material som är utgår från den klassiska perovskitstrukturen kan ha olika funktionella egenskaper och en bred variation av tänkbara applikationer. Några exempel på dessa egenskaper och möjliga applikationer inkluderar god fotokonduktivitet för solceller, utmärkt emissionsegenskaper för ljusdioder och justerbara dielektriska egenskaper för elektroniska växlar och sensorer. De fysiska egenskaperna av det hybrida organiska-oorganiska materialet beror på kristallstrukturen av materialet, som i sig bestäms av valet av komponenter. På grund av de många möjligheter av organiska och oorganiska komponenter så finns det möjlighet att syntetisera helt nya hybrida organiska-oorganiska föreningar som kan ha nya eller förbättrade fysiska egenskaper. Nuvarande hybrida organiska-oorganiska material som utgår från perovskitstrukturen använder huvudsakligen bly som divalent metalkatjon, och det beror på att den ger den bästa funktionella effekten. Blys toxicitet är dock en stor nackdel för nuvarande blybaserade hybrid oorganiska material. Möjligheten att ersätta bly med en annan divalent metall har undersökts under detta projekt. I denna avhandling så har den organiska katjonen cyclohexylammonium (CHA) varit i fokus som den organiska komponenten. Målet med detta examensarbete var att designa, syntetisera och karakterisera nytt hybrid organisk-oorganiskt material. De hybrida organiska-oorganiska föreningarna CHAZnBr3 och (CHA)2ZnBr4 syntetiserades för den första gången, så vitt författaren vet, och kommer vara i fokus i denna avhandling. De två nya hybrida organiska-oorganiska föreningarna blev strukturellt karakteriserade med X-ray Diffraction (XRD) och termiskt karakteriserade med Thermal Gravimetric Analysis (TGA) och Differential Scanning Calorimetry (DSC). Den första föreningen, CHAZnBr3, kunde bestämmas att vara ortorombisk vid 298 K. Föreningen bestämdes vara termisk stabil upp till 490 K, och genomgår en fasövergång vid 445 K. Den andra föreningen, (CHA)2ZnBr4, kunde inte bestämmas strukturellt vid varken 100 K eller 298 K. Föreningen bestämdes vara termisk stabil upp till 490 K, och genomgår en fasövergång vid 230 K. Ytterligare karakterisering krävs för att bättre förstå egenskaperna hos dessa föreningar och deras möjliga användningsområden.The demand for better and more sustainable material is increasing. More efficient materials will be needed to meet the growing global need. Hybrid organic-inorganic materials are one type of materials that have been of great interest recently, which can be described as a class of materials that mix organic and inorganic components. This thesis focused on hybrid organic-inorganic materials inspired by the classical perovskite crystal structure ABX3, where component A is an organic cation, component B is a divalent metal cation and component X is an anion. Hybrid organic-inorganic materials based on the classical perovskite structure may have various functional properties and may have a broad range of potential applications. Some examples of those properties as well as some and possible applications include good photoconductivity and power conversion efficiency for photovoltaic devices, excellent emission properties for light emitting diodes and tunable dielectric properties for electronic switches and sensors. The physical properties of the hybrid organic-inorganic material are determined by the crystal structure of the material, which in turn will be decided by the choice of components. With the many possible choices for organic and inorganic components, there is an opportunity to synthesize completely new hybrid organic-inorganic compounds that may display new or superior physical properties. Current hybrid organic-inorganic materials based on the perovskite crystal structure mainly use lead as the divalent metal, since it currently gives the best performance. The toxicity of lead is a major drawback for current lead-based hybrid organic-inorganic materials. The possibility to replace lead with another divalent metal has been explored during this project. For this thesis, the organic cation cyclohexylammonium (CHA) has been of focus as the organic component. The aim of this thesis was to design, synthesize and characterize novel hybrid organic-inorganic compounds. The hybrid organic-inorganic compounds CHAZnBr3 and (CHA)2ZnBr4 were synthesized for the first time, to the best of our knowledge, and will be the focus of this thesis. The two new hybrid organic-inorganic compounds were structurally characterized by X-ray Diffraction (XRD) and thermally characterized by Thermal Gravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). The first compound, CHAZnBr3, could be determined to be orthorhombic at 298 K. The compound was found to be thermally stable up 490 K, and to undergo a phase transition at 445 K. The second compound, (CHA)2ZnBr4, could not be fully structurally solved at either 100 K or 298 K. The compound was found to be thermally stable up to 490 K, and to undergo a phase transition at 230 K. Further characterization will be needed to better understand the properties of these two compounds and their possible applications.
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Pillar, Rachel Joanne, and rachel pillar@flinders edu au. "The Influence of Rolling Oil Decomposition Deposits on the Quality of 55Al-43.4Zn-1.6Si Alloy Coatings." Flinders University. School of Chemistry, Physics and Earth Sciences, 2007. http://catalogue.flinders.edu.au./local/adt/public/adt-SFU20080108.132120.
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Uncoated defects in hot dip metal-coated steel products result from non-wetting of the steel surface by the molten alloy. The occurrence of uncoated defects is highly detrimental to product quality and production efficiency; uncoated defects compromise the appearance and anti-corrosion performance of hot dip metal-coated steel products and causes time delays in the application of subsequent surface treatments. Although many studies have been directed towards evaluating the effect of steel pre-heat temperature and oxidation on the formation of uncoated defects, fewer investigations have analysed how oil-derived residues remaining on steel surface following the cold rolling and furnace cleaning processes impact upon hot dip metallic coating quality. Furthermore, although a considerable amount of research has focussed on the process of deposit formation in lubricants used in other applications, the composition of oily residues remaining after the continuous annealing process, and the origins of these residues in the original rolling oil formulation, are poorly understood.
The primary focus of the present work has been to gain an improved understanding of relationships between cold rolling oil composition, oil residue-formation characteristics and the occurrence of uncoated defects in 55Al-43.4Zn-1.6Si hot dip metallic coatings. Several key classes of rolling oil ingredients which decompose to leave high levels of thermally-stable residue have been identified. The thermal decomposition processes undergone by a variety ingredients within these classes have been studied under both oxidising and reducing conditions using Thermogravimetric Analysis (TGA) and Pressure Differential Scanning Calorimetry (PDSC) techniques, with chemical characterisation of the decomposition process and the resultant thermally-stable residue by infrared spectroscopy. Model blends of each ingredient in a typical cold rolling oil base ester have also been evaluated by TGA and PDSC to identify the impact of ingredient concentration and chemical structure on the amount of oily residue formed. The results of these investigations have been related to the impact of the ingredients on 55Al-43.4Zn-1.6Si hot dip metallic coating quality through the performance of industrial-scale hot dipping trials and hot dip simulation studies.
In order to translate these results into a context more closely aligned with industrial conditions, the effect of processing variables, including furnace atmosphere and the availability/concentration of iron in contact with the rolling oil at the steel surface, on the decomposition process of a fully-formulated commercial cold rolling oil has also been investigated. The information gained can potentially be used to tailor operating conditions within the cold rolling/continuous hot dip metallic coating processes to enhance steel surface cleanliness.
Finally, the deposit-forming tendencies of an array of different commercial cold rolling oils have been evaluated, leading to the development of a thermal analysis-based test for screening cold rolling oils with respect to their likely impact upon 55Al-43.4Zn-1.6Si hot dip metallic coating quality. This test, together with the understanding obtained on the effect of different rolling oil ingredients on hot dip metallic coating quality, can be used within the industry to formulate improved cold rolling oils.
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Craft, Garrett Michael. "Characterization of Nylon-12 in a Novel Additive Manufacturing Technology, and the Rheological and Spectroscopic Analysis of PEG-Starch Matrix Interactions." Scholar Commons, 2018. http://scholarcommons.usf.edu/etd/7137.
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In this work differential scanning calorimetry, dynamic mechanical analysis, Fourier-Transformed Infrared Spectroscopy [FT-IR] and polarized light microscopy will be employed to characterize polymeric systems. The first chapter broadly covers polymer synthesis and important characterization methods.
In the second chapter, a polyamide (PA12) will be sintered via a novel additive manufacturing (AM) technology developed here at USF termed LAPS (Large Area Projection Sintering). LAPS uses extended sintering timespans to ensure complete melting and densification of the polymer powder over the entire two-dimensional area of the part’s footprint. Further, it allows for the printed layer to crystallize and shrink in its entirety as the temperature falls below the crystallization temperature prior to the next layer being added. The printed parts (termed coupons) will be assayed by DSC and polarized light microscopy to determine sintering efficacy. Additionally, the parts will be compared to coupons printed with conventional methods to show that the USF AM technology shows superior elongation at break (EaB), with comparable ultimate tensile strength (UTS) and Young’s Modulus to laser sintered coupons. This is notable as conventional AM methods produce parts which usually compromise between EaB and modulus. The EaB of LAPS-printed parts is comparable to injection molding (IM) grade PA12, which is remarkable as IM grade PA12 powder normally has higher molecular weight and limited crystallinity. The reduced crystallinity of IM grade PA12 parts is thought to be due to the high shear rates during injection and fast cooling rates post-fabrication. Further, the USF LAPS parts show minimal or no detectable porosity. Porosity is an artifact of the sintering process which conventional techniques like laser sintering (LS) have little ability to mitigate, as higher energy wattages simply burn and degrade the polymer surface with insufficient time available for heat transfer and bulk melt flow. Porosity is documented as one of the leading causes of part failure and decreased mechanical properties in the literature, and as such the USF AM technology is in the process of being patented as of March, 2018.
Chapters three through six will explore a phenomenon first noticed by clinicians at the James A. Haley Veterans Hospital. They observed that starch-thickened drinks for patients suffering from dysphagia became dangerously thinned down upon addition of the osmotic drug polyethylene glycol (PEG) 3350, marketed as Miralax®. Starch-based hydrocolloids are common thickeners used for patients with dysphagia, and so any incompatibility with such a ubiquitous drug as PEG 3350 poses an immediate danger. Patients with the disorder can suffer increased rates of aspiration-related pneumonia, incurring up to nearly a 60% fatality rate within a year. Chances for aspiration greatly increase for food items which are too inviscid to safely swallow. Rheology and FT-IR spectroscopy will be used to show that the breakdown of the starch network in aqueous solution is dependent upon the molecular weight of PEG. As the molecular weight of PEG is reduced to that of a small molecule (~300MW) from its large drug form (3350MW), the structure stabilizes and can resist shearing forces in a steady shear rheological experiment. Spectroscopy will show that PEG molecular weight also influences syneresis and the crystallinity of the starch hydrocolloid solutions.
It is postulated that the molecular weight of PEG influences its miscibility in starch solutions, and its ability to interrupt the hydrogen bonding and entanglements which maintain the elastic framework which allow starch thickeners to impart viscosity and resist shearing forces. When this framework collapses, absorbed water is expelled as evidenced as a biphasic separation where water collects on top of the starch suspension. This was the phenomenon observed by the clinicians at the Veterans’ Hospital.
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Carvalho, Cláudio Teodoro de [UNESP]. "Síntese, caracterização e estudo do comportamento térmico dos 2-metoxibenzoatos de Mn(II), Co(II), Ni(II), Cu(II) e Zn(II) no estado sólido." Universidade Estadual Paulista (UNESP), 2006. http://hdl.handle.net/11449/97865.
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Carbonatos de Mn(II), Co(II), Ni(II), Cu(II) e Zn(II) foram preparados por adição lenta da solução saturada de hidrogeno carbonato de sódio com gotejamento contínuo às soluções dos respectivos cloretos metálicos, exceto para o cobre, até a total precipitação do íon metálico. Os precipitados foram lavados com água destilada para eliminar os íons cloretos e teste qualitativo com solução de AgNO3/HNO3 foi realizado para confirmar a ausência destes, e após isso, foi mantida em suspensão. Os compostos no estado sólido foram preparados pela mistura dos respectivos carbonatos metálicos com o ácido 2-metoxibenzóico (2-MeO-HBz). A suspensão aquosa foi aquecida lentamente próximo da ebulição até neutralização total dos carbonatos. As soluções resultantes depois de arrefecidas foram mantidas em banho de gelo para recristalizar o ácido em excesso e filtradas. Assim, as soluções aquosas dos metoxibenzoatos metálicos foram concentradas em banho maria e o precipitado seco resultante deste processo colocado em um dessecador contendo cloreto de cálcio. O composto de cobre devido a sua baixa solubilidade foi preparado pela adição lenta com gotejamento contínuo de solução do 2-metoxibenzoato de sódio 0.1 mol L-1 à solução de sulfato de cobre, até a total precipitação do íon cobre e o precipitado lavado com água destilada para eliminação do íon sulfato e teste qualitativo de confirmação realizado com BaCl2 0.1 mol L-1, em seguida filtrada em papel de filtro Whatman 40 e o precipitado após seco foi colocado em dessecador contendo cloreto de cálcio. Os compostos sintetizados foram investigados por meio de espectroscopia de infravermelho, difratometria de raio X pelo método do pó, termogravimetria e análise térmica diferencial simultânea (TG-DTA), termogravimetria, termogravimetria derivada (TG/DTG), calorimetria exploratória diferencial (DSC) e outros métodos de análise.
Carbonates of Mn (II), Co (II), Ni (II), Cu (II) and Zn (II) were prepared by adding slowly with continuous stirring saturated sodium hydrogen carbonate solution to the corresponding metal chloride solutions (except copper), until total precipitation of the metal ions. The precipitates were washed with distilled water until elimination of chloride ions (qualitative test with AgNO3/HNO3 solution) and maintained in aqueous suspension. olid state Mn (II), Co (II), Ni (II) and Zn (II) compounds were prepared by mixing the respective metal carbonates with 2-methoxybenzoic acid 99% (2-MeO-HBz) obtained from Aldrich, in slight excess. The aqueous suspension was heated slowly up to near ebullition, until total neutralization of the respective carbonates. The resulting solutions after cooled were maintained in an ice bath to recrystallize the acid in excess and filtered through a Whatman nº 40 filter paper. Thus, the aqueous solutions of the respective metal 2-methoxybenzoates were evaporated in a water bath until near dryness and kept in a desiccator over calcium chloride. The copper compound due to its low solubility was prepared by adding slowly, with continuous stirring, the aqueous solution of Na-2-MeO-Bz 0.1 mol L-1 to the respective metal sulphate solution, until total precipitation of the metal ions. The precipitate was washed with distilled water until elimination of the sulphate ion, filtered through and dried on Whatman no42 filter paper, and kept in a desiccator over anhydrous calcium chloride, under reduced pressure to constant mass. The compounds were investigated by means of infrared spectroscopy, X-Ray powder diffractometry, simultaneous thermogravimetry and differential thermal analysis (TG-DTA), Thermogravimetry derivative termogravimetry (TG/DTG), differential scanning calorimetry (DSC) and other methods of analysis.
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Ramos, Júnior Fernando José de Lima. "Classificação de analgésicos utilizando técnica espectroscópica e termoanalítica associadas a métodos quimiométricos." Universidade Estadual da Paraíba, 2014. http://tede.bc.uepb.edu.br/tede/jspui/handle/tede/2320.
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In the last years occurred a significant increase in the use of analgesics, for example, those that contain acetaminophen as the active pharmaceutical ingredient, being essential for the pharmaceutical industry and the supervisory organs a rigorous control in the production of these medicines. Thus, it becomes necessary the improvement of techniques with the application of reliable analytical methodologies, which are, preferably, quick and low cost, as, for example, the Near Infrared (NIR) Spectroscopy and the Differential Scanning Calorimetry (DSC). Though, even being techniques with extensive analytical power, its use is hampered in samples such as medicines, because results are presented in a complex way for direct interpretation, making the use of chemometric methods necessary. In this context, the objective of this study was to analyze by differential scanning calorimetry and by near infrared spectroscopy, combined with multivariate chemometric techniques, medicines containing acetaminophen and caffeine. So, three brands of medicines were analyzed by DSC and two classes of medicines by NIR. Having the DSC curves obtained in nitrogen atmosphere (50 mL min -1 ), in the temperature range from 92.00 to 190.00 °C, with heating rate of 10 ° C min -1 and preprocessed with the technique Standard Normal Variate (SNV), and the NIR spectra obtained in the interval from 1950 to 2500 nm and preprocessed employing the first derivative, with the filter Savitzky-Golay, second order polynomial and window of 19 points. Posteriorly, it was performed the analgesics classification using the models Linear Discriminant Analysis (LDA) with Successive Projection Algorithm (SPA) and with Genetic Algorithm (GA-LDA) as variable selection techniques, and the K-Nearest Neighbor (KNN), in addition, the DSC curves data were also submitted to Principal Components Analysis (PCA). It was observed for the data obtained by DSC, that the PCA separated the brand M3 of M1 and M2; SPA-LDA and GA-LDA presented a success rate of 94.74 % for the training set and 90,00 % for the test set and the KNN method classified the samples with 100 % of success. On the other hand, for those obtained by NIR, in the SPA-LDA model the success rate was 97.77 % and 84.44 %, in the GA-LDA 96.66 % and 93.33 %, and in the KNN method 100 % and 80 %, for training set and test set, respectively. Thereby, the analysis of the obtained results showed that DSC and NIR techniques aggregate to chemometric methods are efficient alternatives to the use of High Performance Liquid Chromatography (HPLC), with the advantage of achieving results quickly, low cost and without generating pollutant residues, making feasible the use of these techniques to streamline the quality control in pharmaceutical industries, as well as, to assist the surveillance authorities in the rapid detection of medicines adulteration.
Nos últimos anos ocorreu um aumento significativo no uso de analgésicos, por exemplo, aqueles que contêm o paracetamol como ingrediente ativo farmacêutico, sendo indispensável para a indústria farmacêutica e os órgãos de fiscalização um rigoroso controle na produção desses medicamentos. Para tanto, faz-se necessário o aprimoramento das técnicas com aplicação de metodologias analíticas confiáveis, que sejam, de preferência, rápidas e de baixo custo, como, por exemplo, a Espectroscopia no Infravermelho Próximo (NIR) e a Calorimetria Exploratória Diferencial (DSC). Entretanto, mesmo essas técnicas possuindo amplo poder analítico, sua utilização é dificultada em amostras como medicamentos, pois os resultados apresentam-se complexos à interpretação direta, fazendo-se necessário o uso de métodos quimiométricos. Nesse contexto, o objetivo desse trabalho foi analisar por calorimetria exploratória diferencial e por espectroscopia no infravermelho próximo, associadas a técnicas quimiométricas multivariadas, medicamentos a base de paracetamol e cafeína. Por isso, analisaram-se três marcas de medicamentos por DSC e duas classes de medicamentos por NIR. Tendo as curvas de DSC obtidas em atmosfera de nitrogênio (50 mL min -1 ), na faixa de temperatura de 92,00 a 190,00 ºC, com razão de aquecimento de 10 ºC min -1 e pré-processadas com a técnica de Padrão Normal de Variação (SNV), e os espectros NIR obtidos num intervalo de 1.950 a 2.500 nm e pré-processados empregando-se a primeira derivada, com o filtro de Savitzky-Golay, polinômio de segunda ordem e janela de 19 pontos. Posteriormente, realizou-se a classificação dos analgésicos pelos modelos Análise Discriminante Linear (LDA) com Algoritmo das Projeções Sucessivas (SPA-LDA) e com Algoritmo Genético (GA-LDA) como técnicas de seleção de variáveis, e com o K-ésimo Vizinho Mais Próximo (KNN), além desses, os dados das curvas DSC também foram submetidos a Análise de Componentes Principais (PCA). Observou-se para os dados obtidos por DSC, que a PCA separou a marca M3 de M1 e M2; o SPA-LDA e GA-LDA apresentaram índice de acerto de 94,74 % para o conjunto de treinamento e 90,00 % para o conjunto de teste e o método KNN classificou as amostras com 100 % de sucesso. Por outro lado, para aqueles obtidos por NIR, no modelo SPA-LDA a taxa de acerto foi 97,77 % e 84,44 %; no GA-LDA 96,66 % e 93,33 %; e no método KNN 100 e 80 %, para o conjunto de treinamento e o de teste, respectivamente. Desse modo, a análise dos resultados obtidos permitiu inferir que as técnicas DSC e NIR associadas a métodos quimiométricos são alternativas eficientes ao uso da Cromatografia Líquida de Alta Eficiência (CLAE), com a vantagem de alcançarem resultados com rapidez, baixo custo e sem geração de resíduos poluentes, o que torna viável a utilização dessas técnicas para agilizar o controle da qualidade nas indústrias farmacêuticas, bem como, para auxiliar os órgãos de fiscalização na detecção rápida de adulterações em medicamentos.
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Cristofolini, Renato. "Estudo da potencialidade da aplicação do ferro fundido nodular ASTM A536 60-40-18 como materia prima para processos de tixoconformação." [s.n.], 2009. http://repositorio.unicamp.br/jspui/handle/REPOSIP/263560.
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Orientador: Maria Helena RobertTese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecanica
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Resumo: Este trabalho analisa a tixohabilidade, a viabilidade de produção de pastas tixotrópicas e as transformações de fase que ocorrem na tixofundição do ferro fundido nodular ASTM A536 60-40-18. A análise da tixohabilidade é feita através de análises térmicas utilizando técnicas de Análise Térmica Diferencial (ATD) e Calorimetria Exploratória Diferencial (CED) em diferentes condições operacionais (tipo de ciclo e taxas de aquecimento/resfriamento), e através de simulação termodinâmica utilizando software THERMOCALC®. São discutidas a influência das condições dos ensaios nas temperaturas de transformações e intervalos de solidificação, e os resultados comparados com os obtidos por simulação. São discutidas as transformações de fases que ocorrem e as respectivas temperaturas, sendo proposto diagrama de fases para a liga específica em estudo. São determinadas a sensibilidade da variação da fração líquida com a temperatura (dFL/dT) e sugeridas janelas de tixoconformação, para todas as condições analisadas. Os resultados obtidos indicam uma faixa de operação para a tixoconformação da ordem de 20oC, onde uma transformação eutética se faz presente e a variação da fração líquida com a temperatura pode ser controlada adequadamente. A janela de tixoconformação depende da taxa de transferência de calor empregada: quanto maior a taxa, maior o intervalo de transformação eutética e maior a janela de tixoconformação. Quanto à análise da viabilidade de produção de pastas tixotrópicas, foram produzidas pastas por fusão parcial controlada a distintas temperaturas dentro da faixa de operação para tixoconformação determinada previamente. As microestruturas resultantes foram analisadas por microscopia ótica (MO) e eletrônica de varredura (MEV), difratometria de raios-x e microanálise utilizando energia dispersiva (EDS). Os resultados mostram a viabilidade de produção de pastas com características tixotrópicas, nas condições analisadas, apesar da estreita faixa de temperaturas da janela de tixoconformação do material estudado. Mostram ainda que a temperatura de tratamento influencia a quantidade e dimensões dos nódulos de grafita presentes na matriz da pasta, sendo que temperaturas de tixofundição superiores à faixa de transformação eutética podem levar à rápida dissolução desses nódulos e como consequência, o aumento da dureza da liga e redução de sua ductilidade. O produto tixofundido apresenta, à temperatura ambiente, estrutura constituída essencialmente de martensita, resultado do resfriamento rápido da austenita, grafita nodular de pequenas dimensões e de fases complexas em contornos de grãos martensíticos.
Abstract: This work analyses the thixoability, the viability of actual production of thixotropic semi-solid of ferritic nodular cast iron ASTM A536 60-40-18, as well as the phase transformations taking place in the process. Thixoability evaluation is made through thermal analysis by Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC) tests in different conditions (cycle type and heating/cooling rate), and also through thermodynamic simulations using THERMOCALC® software. Related to these analysis it is evaluated the influence of tests conditions on transformations temperatures and ranges; results are compared to those obtained by simulation. Phase transformations are discussed and a specific phase diagram for the alloy investigated is proposed. Liquid fraction sensitivities with temperature (dFL/dT) are determined, and thixoforming windows are suggested. Results indicate that a thixoforming window in the order of 20°C are available; in this range a eutectic transformation takes place and the liquid fraction can be controlled. Beyond the eutectic temperature liquid fraction increases significantly with temperature variation and processing control can not be assured. Thixoforming windows depend on heat transfer rates: higher the rate, higher the eutectic range and the thixoforming window. To analyse the viability of actually producing thixotropic slurries by partial melting, samples were heated to temperatures within the thixoforming windows previously suggested. Resulting microstructures were analysed by optical and electronic microscopy, X-R diffraction and EDS microanalysis. Results show the feasibility of producing thixotropic semi-solid of the studied nodular iron, in spite of its narrow thixoforming field; treatment temperature influences the size and amount of graphite nodules in the matrix. Higher temperatures can lead to fast dissolution of graphite, jeopardizing the ductility of the material. Thixocast product presents, at room temperature, small nodules of graphite in a martensitic matrix and a complex phase in grain boundaries.
Doutorado
Materiais e Processos de Fabricação
Doutor em Engenharia Mecânica
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Gul, Kiymet Gizem. "Thermal Characterization And Kinetic Analyis Of Sara Fractions Of Crude Oils By Tga And Dsc Methods." Master's thesis, METU, 2011. http://etd.lib.metu.edu.tr/upload/12613614/index.pdf.
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In this thesis, four different crude oil samples and their saturate, aromatic and resin fractions were analyzed by two different thermoanalytical methods, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The experiments were performed at three different heating rates (5, 10 and 15 °C/min) under air atmosphere. Same gas flow rate and same pressure were applied to all samples. The aim is to determine the kinetic analysis and combustion behavior of crude oils and their fractions and also determining the effect of heating rate on all samples. For all samples two main reaction regions were observed in thermogravimetry (TG), differential thermogravimetry (DTG) and DSC curves due to the oxidative degradation of crude oil components. It was deduced that the free moisture, volatile hydrocarbons were evaporated from the crude oils, light hydrocarbons were burned and fuel was formed in the first reaction region. The second reaction region was the main combustion region where the fuel was burned. From the TGA curves, it was detected that the heavier fraction, resins, lost considerable amounts of their initial mass, approximately 35%, while saturates lost only approximately 3% of their initial mass in the second reaction region. DSC curves of the samples were also examined and observed that as the sample got heavier, the heat of the reaction increased. Saturates, lightest part of the crude oil fractions, gave minimum heat of reaction. As the heating rate increased, shift of peak temperatures to high values and higher reaction regions were observed. The kinetic analysis of crude oils and their fractions were also performed using different kinetic methods. Activation energies (E), mean activation energies (Emean) and Arrhenius constants were found for crude oils and fractions. It was deduced that the resins gave the highest activation energy and Arrhenius constant for both reaction regions. Moreover, it was encountered that heating rate has no effect on activation energies.
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Batisai, Eustina. "Synthesis and sorption studies of porous metal-organic hosts." Thesis, Stellenbosch : Stellenbosch University, 2013. http://hdl.handle.net/10019.1/79803.
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Thesis (PhD)--Stellenbosch University, 2013.ENGLISH ABSTRACT: The first part of this study describes the synthesis of new porous materials from basic building blocks. Five structurally related ligands namely: N,N'-bis(3-pyridylmethyl)-naphthalene diimide (L1), N,N'-bis(4-pyridylmethyl)-naphthalene diimide (L2), N,N'-bis(4-pyridylmethyl)- pyromellitic diimide (L3), N,N'-bis(3-pyridylmethyl)-pyromellitic diimide (L4) and 2-(pyridin-4- ylmethyl)-benzene tricarboxylic anhydride (L5) were synthesised. Ligands L1 and L2 were reacted with metal nitrates and carboxylates as co-ligands in a systematic manner with a view to obtaining potentially porous 3–D coordination polymers. Ten structurally diverse coordination polymers were obtained and they were characterised by single-crystal X-ray diffraction, powder X-ray diffraction and thermogravimetric analysis. Four of these compounds absorb moderate amounts of CO2 and, in addition, show sorption selectivity towards CO2 over N2. The reaction of L3 and L4 with transition metal halides yielded two 1–D chains, while the reaction of L5 with transition metal nitrates yielded seven coordination polymers of which four are 2–D and three are 1–D. Of the 2–D structures three are isostructural. The second part of this work describes a variable pressure study of a flexible metal-organic framework [Zn2(BDC)2(BPY)] (BPY = 4,4 -bipyridine and BDC = 1,4-benzene dicarboxylic acid). [Zn2(BDC)2(BPY)] is one of the few examples of a flexible metal-organic framework that undergoes phase transformations in response to gas pressure. The high pressure sorption recorded for this metal-organic framework displays two inflection steps in the pressure range 0 to 30 bar, possibly indicating two phase transformations. The gas-loaded structures for each phase transformation were determined by means of single-crystal X-ray diffraction. High-pressure differential scanning calorimetry was also carried out on the system in order to determine accurate gate-opening pressures, as well as the energies involved with each phase transformation. The results correlate with those obtained from single-crystal X-ray diffraction and high-pressure sorption. The final section reports the mechanochemical synthesis of two Werner complexes [NiCl2(4- PhPy)4] (1), [CoCl2(4-PhPy)4] (2) and their corresponding solid solution [Ni0.5Co0.5Cl2(4-PhPy)4] (3) (PhPy = phenyl pyridine). The solid solution could only be formed by mechanochemical synthesis and not by conventional solution crystallisation methods. The solid solution exhibits sorption properties that differ from those of the pure compounds.
AFRIKAANSE OPSOMMING: Die eerste deel van hierdie studie beskryf die sintese van nuwe poreuse stowwe uit basiese boublokke. Vyf struktureel verwante ligande naamlik: N,N'-bis(3-piridielmetiel)-naftaleen diimied (L1), N,N'-bis(4-piridielmetiel)-naftaleen diimied (L2), N,N'-bis(4-piridielmetiel)- piromellitien diimied (L3), N,N'-bis(3-piridielmetiel)-piromellitien diimied (L4) en 2-(piridiel-4- ielmetiel)benseen trianhidried (L5) is gesintetiseer. Ligande L1 en L2 is gereageer met metaal nitrate en karboksielsure as mede-ligande in 'n sistematiese wyse met 'n oog op die verkryging van potensieel poreuse 3–D koördinasie polimere. Tien struktureel diverse koördinasie polimere is verkry en hulle is gekarakteriseer deur enkel-kristal X-straal-diffraksie, poeier X-straal diffraksie en termo-analise (thermal analysis). Vier van hierdie verbindings het matige hoeveelhede CO2 geabsorbeer en, bykomend, wys sorpsie selektiwiteit van CO2 oor N2. Die reaksie van L3 en L4 met oorgangsmetaalhaliede het twee 1–D kettings gevorm, terwyl die reaksie van L5 met oorgangsmetaal nitrate sewe koördinasie polimere opgelewer het, waarvan vier 2–D en drie 1–D polimere is. Van die 2–D polimere het drie vergelykbare strukture. Die tweede deel van hierdie werk beskryf 'n veranderlike druk studie van 'n buigsame metaalorganiese raamwerk [Zn2(BDC)2(BPY)] (BPY = 4,4-bipiridien en BDC = 1,4-benseen dikarboksielsuur). [Zn2(BDC)2(BPY)] is een van die min voorbeelde van 'n buigsame metaalorganiese raamwerk wat fase transformasies (phase transformations) ondergaan in respons op ‘n verandering in gas druk. Die hoë-druk sorpsie aangeteken vir hierdie metaal-organiese raamwerk vertoon twee infleksie stappe in die gebestudeerde druk gebied (0 tot 30 bar), wat moontlik op twee fase transformasies dui. Die gas-gelaaide strukture vir elke fase transformasie is bepaal deur middel van enkel-kristal X-straal-diffraksie. Hoë-druk differensiële skandeer kalorimetrie (differential scanning calorimetry) is ook uitgevoer op die stelsel ten einde dié akkurate hekopenings druk, sowel as die energie betrokke by elke fase transformasie te bepaal. Die resultate stem ooreen met dié verkry vanaf enkel-kristal X-straal diffraksie en hoë-druk sorpsie. Die finale afdeling bespreek die meganochemiese sintese van twee Werner komplekse [NiCl2(4-PhPy)4] (1) en [COCl2(4-PhPy)4] (2) en hul ooreenstemmende vaste oplossing (solid solution) [Ni0.5Co0.5Cl2(4-PhPy)4] (3). Die vaste oplossing kan slegs gevorm word deur meganochemiese sintese en nie deur konvensionele oplossing kristallisasie metodes. Die vaste oplossing vertoon sorpsie eienskappe wat verskil van dié van die suiwer verbindings.
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Carvalho, Tânia Isabel da Silva. "Development of ion jelly thin films for electrochemical devices." Doctoral thesis, Faculdade de Ciências e Tecnologia, 2013. http://hdl.handle.net/10362/10874.
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Dissertação para obtenção do Grau de Doutor em Química SustentávelIonic liquids (ILs) are promising materials which have been used in a wide range of applications. However, their major limitation is their physical state. In order to address this challenge, a self-supported IL-based material was developed by combining gelatine with an IL, originating a quasi-solid material named Ion Jelly (IJ). This is a light flexible material, dimensionally stable, with promising properties to develop safe and highly conductive electrolytes. This thesis is focused on the characterization of IJ films based on different ILs. The conductive mechanisms of IJ materials were studied using dielectric relaxation spectroscopy (DRS) in the frequency range 10-1−106 Hz. The study was complemented by differential scanning calorimetry (DSC) and pulsed field gradient nuclear magnetic resonance (PFG NMR) spectroscopy. A glass transition was detected by DSC for all materials allowing to classify them as glass formers. From dielectric measurements, transport properties such as mobility and diffusion coefficients were extracted. Moreover, it was found that the diffusion coefficients and mobility are similar for the IL and IJ, especially for the IL EMIMDCA. Since for BMIMDCA, those properties significantly change upon hydration, the influence of water content [0.4 - 30% (w/w)] was also studied for the ILs. In particular for BMPyrDCA with 30% water, it was analyzed the reorientational polarization by the complex permittivity and electric modulus, from which three different processes were identified: a secondary relaxation with Arrhenian temperature dependence, the process that is believed to be behind the dynamic glass transition and the mobility of charge carriers. An application of the IJs was successfully explored with a chemoresistive gas sensor made up by different IJs as active layer, which is an electronic nose formed by an array of such sensors. The performance of this e-nose revealed its ability to correctly detect eight common volatile solvents.
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Lans, Alexa Michelle. "Evaluation of Water Sorption and Thermal Properties of Galacto-oligosaccharides, and Application in Glassy Confections." The Ohio State University, 2016. http://rave.ohiolink.edu/etdc/view?acc_num=osu1460764786.
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Smith, Beverly. "Investigating Thermal Transformations of Ligand-Stabilized Gold Nanoparticles: Influence of the Structural Attributes of the Nanoparticle and Its Environment on Thermal Stability." Thesis, University of Oregon, 2015. http://hdl.handle.net/1794/19259.
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Ligand-stabilized metal nanoparticles (LSNPs) have garnered significant attention for use in applications including sensing, catalysis, and thin film fabrication. Many uses rely on the size-dependent properties of the metal nanoparticle core. Therefore, preservation of nanoparticle core size is of paramount importance. In other uses, the low processing temperatures afforded by metal LSNPs make them attractive as precursors for conductive thin films. In these distinctly different applications, understanding nanoparticle thermal stability is crucial.
A key finding of this research is that nanoparticle sintering is dependent upon both core size and ligand functionality. Multi-technique analysis of four types of gold nanoparticles (AuNPs) with different ligand compositions and core sizes illustrates that more volatile ligands reduce the onset temperature for sintering. Also, AuNPs of larger core size with the same ligand composition exhibit lower sintering onset temperatures. Correlation between measurements reveals that only a small amount of ligand loss is necessary to trigger rapid sintering and that ligands are excluded to the surface of the porous gold films.
AuNPs with ligand shells composed of two alkanethiols of different chain length and volatility indicate that the onset temperature of sintering can be tuned further through incorporation of a small amount of more volatile alkanethiol into a ligand shell of lower volatility. Mixed LSNPs further reveal that AuNP thermal stability depends upon the ligand shell composition and its intermolecular interactions, which can result in markedly different sintering behavior for different ligand compositions. Long-chain alkanethiol AuNPs sinter after only a small amount of ligand loss, whereas short-chain alkanethiol AuNPs sinter following complete ligand loss and the formation of metastable bare AuNPs. Heated AuNP films prepared with mixed-ligand AuNPs exhibit ligand-dependent differences in film morphology.
To probe AuNP thermal stability in 2D-assemblies, self-assembly using larger ‘marker’ nanoparticles enables the study of small 1.5 nm AuNP arrays with successive TEM monitoring throughout ex situ heating. Monitoring images of the same area shows short-range (1-2 nm) nanoparticle migration/coalescence. In contrast to 3D assemblies, AuNP growth occurs at temperatures as low as 60 °C.
This dissertation includes previously published and unpublished co-authored material.10000-01-01
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Chbeir, Ralph. "Correlating Melt Dynamics with Topological Phases of Homogeneous Chalcogenide- and Modified Oxide- Glasses Using Raman Scattering, Infra-Red Spectroscopy, Modulated-Differential Scanning Calorimetry and Volumetric Experiments." University of Cincinnati / OhioLINK, 2019. http://rave.ohiolink.edu/etdc/view?acc_num=ucin1573224465185235.
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