As part of the production of certain solid-dosage pharmaceuticals, granulated ingredients are dried in a batch fluidized bed dryer. Currently, the determination of the completion of the drying process is accomplished through measurements of product or outlet air temperatures. No quantitative measurement of hydrodynamic behaviour is employed. Changes in bed hydrodynamics caused by variations in fluidization velocity may lead to increased particle attrition. In addition, excessive desiccation of the granules caused by inaccurate determination of the drying endpoint may lead to an increase in the thermal and mechanical stresses within the granules. The activity of future high-potency or peptide based drug products may be influenced by these effects. Therefore, the quantification of hydrodynamic changes may be a key factor in the tighter control of both fluidization velocity and product moisture, which are critical for maintaining product quality. <p>High-frequency measurements of pressure fluctuations in a batch fluidized bed dryer containing pharmaceutical granulate have been used to provide a global, non-intrusive indication of the hydrodynamic changes occurring throughout the drying process. A chaotic attractor comparison statistical test known as the S-statistic, has been applied to quantify these changes in drying and a related unit operation, fluidized bed granulation. The S-statistic showed a sensitivity to moisture which is not seen with frequency and amplitude analysis. In addition, the S-statistic has been shown to be useful in identifying an undesirable bed state associated with the onset of entrainment in a bed instrumented for the collection of both pressure fluctuation and entrainment data. Thus, the use of the S-statistic analysis of pressure fluctuations may be utilized as a low-cost method for determining product moisture or changes hydrodynamic state during fluidized bed drying. <p>Electrical capacitance tomography (ECT) has also been applied in this study to image the flow structure within a batch fluidized bed used for the drying of pharmaceutical granulate. This represents the first time that ECT has been applied to a bed of wet granulate material. This was accomplished through the use of a novel dynamic correction technique which accounts for the significant reduction in electrical permittivity occurring as moisture is lost during the drying process. The correction has been independently verified using x-ray tomography. <p>Investigation of the ECT images taken in the drying bed indicates centralized bubbling behaviour for approximately the first 5 minutes of drying. This behaviour is a result of the high liquid loading of the particles at high moisture. Between moisture contents of 18-wt% and 10-wt%, the tomograms show an annular pattern of bubbling behaviour with a gradual decrease in the cross-sectional area involved in bubbling behaviour. The dynamic analysis of this voidage data with the S-statistic showed that a statistically significant change occurs during this period near the walls of the vessel, while the centre exhibits less variation in dynamic behaviour. The changes identified by the S-statistic analysis of voidage fluctuations near the wall were similar to those seen in the pressure fluctuation measurements. This indicates that the source of the changes identified by both these measurement techniques is a result of the reduction in the fraction of the bed cross-section involved in bubbling behaviour. At bed moisture contents below 5-wt%, rapid divergence was seen in the S-statistic applied to both ECT and pressure fluctuation measurements. This indicates that a rapid change in dynamics occurs near the end of the drying process. This is possibly caused by the entrainment of fines at this time, or the build-up of electrostatic charge. <p>The use of the complimentary pressure fluctuation and ECT measurement techniques have identified changes occurring as a result of the reduction of moisture during the drying process. Both the localized changes in the voidage fluctuations provided by the ECT imaging and the global changes shown by the pressure fluctuation measurements indicate significant changes in the dynamic behaviour caused by the reduction of moisture during the drying process. These measurement techniques could be utilized to provide an on-line indication of changes in hydrodynamic regime. This information may be invaluable for the future optimization of the batch drying process and accurate determination of the drying endpoint.

As part of the production of certain solid-dosage pharmaceuticals, granulated ingredients are dried in a batch fluidized bed dryer. Currently, the determination of the completion of the drying process is accomplished through measurements of product or outlet air temperatures. No quantitative measurement of hydrodynamic behaviour is employed. Changes in bed hydrodynamics caused by variations in fluidization velocity may lead to increased particle attrition. In addition, excessive desiccation of the granules caused by inaccurate determination of the drying endpoint may lead to an increase in the thermal and mechanical stresses within the granules. The activity of future high-potency or peptide based drug products may be influenced by these effects. Therefore, the quantification of hydrodynamic changes may be a key factor in the tighter control of both fluidization velocity and product moisture, which are critical for maintaining product quality. <p>High-frequency measurements of pressure fluctuations in a batch fluidized bed dryer containing pharmaceutical granulate have been used to provide a global, non-intrusive indication of the hydrodynamic changes occurring throughout the drying process. A chaotic attractor comparison statistical test known as the S-statistic, has been applied to quantify these changes in drying and a related unit operation, fluidized bed granulation. The S-statistic showed a sensitivity to moisture which is not seen with frequency and amplitude analysis. In addition, the S-statistic has been shown to be useful in identifying an undesirable bed state associated with the onset of entrainment in a bed instrumented for the collection of both pressure fluctuation and entrainment data. Thus, the use of the S-statistic analysis of pressure fluctuations may be utilized as a low-cost method for determining product moisture or changes hydrodynamic state during fluidized bed drying. <p>Electrical capacitance tomography (ECT) has also been applied in this study to image the flow structure within a batch fluidized bed used for the drying of pharmaceutical granulate. This represents the first time that ECT has been applied to a bed of wet granulate material. This was accomplished through the use of a novel dynamic correction technique which accounts for the significant reduction in electrical permittivity occurring as moisture is lost during the drying process. The correction has been independently verified using x-ray tomography. <p>Investigation of the ECT images taken in the drying bed indicates centralized bubbling behaviour for approximately the first 5 minutes of drying. This behaviour is a result of the high liquid loading of the particles at high moisture. Between moisture contents of 18-wt% and 10-wt%, the tomograms show an annular pattern of bubbling behaviour with a gradual decrease in the cross-sectional area involved in bubbling behaviour. The dynamic analysis of this voidage data with the S-statistic showed that a statistically significant change occurs during this period near the walls of the vessel, while the centre exhibits less variation in dynamic behaviour. The changes identified by the S-statistic analysis of voidage fluctuations near the wall were similar to those seen in the pressure fluctuation measurements. This indicates that the source of the changes identified by both these measurement techniques is a result of the reduction in the fraction of the bed cross-section involved in bubbling behaviour. At bed moisture contents below 5-wt%, rapid divergence was seen in the S-statistic applied to both ECT and pressure fluctuation measurements. This indicates that a rapid change in dynamics occurs near the end of the drying process. This is possibly caused by the entrainment of fines at this time, or the build-up of electrostatic charge. <p>The use of the complimentary pressure fluctuation and ECT measurement techniques have identified changes occurring as a result of the reduction of moisture during the drying process. Both the localized changes in the voidage fluctuations provided by the ECT imaging and the global changes shown by the pressure fluctuation measurements indicate significant changes in the dynamic behaviour caused by the reduction of moisture during the drying process. These measurement techniques could be utilized to provide an on-line indication of changes in hydrodynamic regime. This information may be invaluable for the future optimization of the batch drying process and accurate determination of the drying endpoint.

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No description available.

Introdução: A comprovação da eficiência de formulações hidratantes deve ser criteriosa e analisada com métodos adequados. Objetivo: O objetivo principal do trabalho foi avaliar in vivo a eficácia hidratante de formulações contendo diferentes componentes ativos por capacitância elétrica e perda de água transepidérmica. Compararam-se os desempenhos entre Corneometer® e Moisturemeter® e entre o Vapometer® e Tewlmeter®. Verificou-se o comportamento in vitro das alterações causadas pelas substâncias hidratantes, em modelo de estrato córneo alternativo. Material e Métodos: Os compostos ativos selecionados (4% p/p) para incorporação nos géis à base de carbômero foram: uréia, extrato vegetal de Imperata cylindrica; complexo contendo fatores de hidratação natural; e os derivados do açúcar, sacarídeo isomerato e a mistura de xilitilglicosídeo e anidroxilitilglicosídeo. A avaliação in vivo da eficácia hidratante teve o delineamento experimental baseado no projeto fatorial ANOVA three way. Os tempos estudados foram: após a aplicação e 30, 60, 120; 240 e 360 minutos. O estudo de estabilidade acelerada das formulações envolveu condições drásticas de armazenamento (temperatura, umidade e luminosidade) durante 90 dias. Na avaliação in vitro do comportamento das substâncias hidratantes utilizou-se a espectroscopia Raman com transformada de Fourier (FT-Raman) e Calorimetria exploratória diferencial (DSC). Resultados: A análise estatística da capacitânia elétrica obtida por Corneometer® e do Moisturemeter® mostraram que houve diferenças significativas entre os géis e o tempo de aplicação. Com relação às medidas de perda de água transepidérmica, os resultados obtidos por Vapometer® e Tewlmeter® não apresentaram concordância. As bandas encontradas nos espectros FT-Raman mostraram que os ativos hidratantes não provocaram alterações na estrutura conformacional do estrato córneo alternativo. A análise da calorimetria (DSC) mostrou que o gel de uréia aumentou o conteúdo hídrico da membrana. Conclusão: Os géis contendo 4% (p/p) de uréia e de 4% (p/p) de derivado de açúcar apresentaram melhor eficácia hidratante in vivo, capacitância elétrica quando analisado por Corneometer® e Moisturemeter®. Em relação à perda de água transepidérmica, o gel base sem ativo obteve o melhor resultado. Com relação às medidas de capacitância, o Corneometer® e o Moisturemeter® mostraram-se estaticamente semelhantes. Comparando-se as medidas de perda de água transepidérmica, a análise estatística indicou que o Vapometer® tem precisão inferior comparada com o Tewlmeter®. A avaliação do comportamento in vitro das substâncias hidratantes sugeriram que as mesmas são seguras. / Introduction: Hydration of the corneal layer varies according to the amount of water present; the transportation of water from the lower layers; evaporation speed and quantity and composition of epicutaneous emulsion. Proof of moisturizer formula efficiency must be prudent and analyzed using appropriate methods. Objective: The studys main objective was to assess the in vivo efficacy of moisturizer formulas with different active components by means of electrical capacitance and transepidermal water loss. The accelerated stability of the referred to formulas was also observed and assessed. Performances between Corneometer® and Moisturemeter® and between Vapometer® and Tewlmeter® were compared. In vitro behavior of alterations caused by moisturizing substances was verified in an alternative corneal stratum model. Material and Methods: The active compounds selected (4% p/p) for use in carbomer-based gels were: urea, Imperata cylindrica vegetal extract; a complex with natural moisturizing factors; sugar byproducts, saccharide isomerate and the mix of xylitol glucoside and anhydro xylitol glicoside. In vivo assessment of moisturizing efficacy of the formulas by means of electrical capacitance and transepidermal water loss was designed based in ANOVA three way factorial design. The gels were applied on both arms of volunteers aged 20 to 30 and a control application (base gel) and an untreated area were used. Study times were: after application and at 30, 60, 120; 240 and 360 minutes. The accelerated stability study of the formulations involved drastic storage conditions (temperature, humidity, luminosity) over 90 days. For the in vitro assessment of moisturizing substance behavior, Raman spectroscopy was used with Fourier Transform (FT-Raman) and differential scanning calorimetry (DSC). Results: Statistical analysis of electrical capacitance using Corneometer® and Moisturemeter® revealed significant differences between the gels and application time. With regard to transepidermal water loss measures, the results obtained from Vapometer® and Tewlmeter® did not reveal concordance. The bands found in the FT-Raman spectrum revealed that the active moisturizers did not cause changes in the alternative cornea stratum conformation structure. Calorimetry (DSC) analysis showed the urea gel increased membrane water content. Conclusion: Gels containing 4% (p/p) urea and 4% (p/p) of sugar byproduct had the best in vivo moisturizing efficacy, electrical capacitance when analyzed with Corneometer® and Moisturemeter®. In relation to transepidermal water loss, the base gel without active ingredients had the best result in both Vapometer® and Tewlmeter®. The formulas were stable for a period of three months in the studied storage conditions. In relation to capacitance measures, Corneometer® and Moisturemeter® proved to be statistically similar. When comparing transepidermal water loss measures, statistical analysis indicated that Vapometer® is not as precise as Tewlmeter®. In vitro assessment of behavior of moisturizing substances suggested they are safe.

Made available in DSpace on 2015-05-08T15:00:00Z (GMT). No. of bitstreams: 1 parte1.pdf: 2338507 bytes, checksum: 6275f329bc4f4dc275a86cd47c9ba994 (MD5) Previous issue date: 2009-04-30 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / This thesis aims to computationally simulate the electronic transducer for a parallel electrical capacitance tomography, can generate a voltage level used for image reconstruction of the adsorption phenomenon occurred in the adsorptive bed. This simulation was performed using a computer program like SPICE (Simulation Program with Integrated Circuit Emphasis) for the purpose of defining the parameters for its construction, dedicated to the application of the adsorptive bed bench in a glass case studies of the adsorptive process. This technique uses capacitive sensors coupled to an electronic transducer that will generate a voltage signal associated with the distribution of dielectric permittivity of the medium. The simulation is developed to simulate the main circuit, a differentiator, fitted with high frequency OPA 2690. The simulated model is a simple circuit with a transmitter and a receiver. The results show the technical feasibility of the project being proposed for future work to implement a prototype of the electronic transducer of electrical capacitance tomography applied to the study of the adsorption process. / Esta dissertação tem como objetivo simular computacionalmente o transdutor eletrônico para um tomógrafo capacitivo elétrico paralelo capaz de gerar um nível de tensão utilizado para a reconstrução da imagem do fenômeno de adsorção ocorrido no leito adsortivo. Esta simulação foi realizada em um programa computacional do tipo SPICE (Programa de Simulação com Ênfase em Circuito Integrado) com a finalidade de definir os parâmetros para a sua construção, voltado para a aplicação no leito adsortivo de uma bancada em vidro para estudos do processo adsortivo. Esta técnica utiliza sensores capacitivos acoplados a um transdutor eletrônico que vão gerar um sinal de tensão associado à distribuição da permissividade dielétrica do meio. A simulação desenvolvida consiste em simular o circuito principal, um diferenciador, montado com OPA 2690 de alta freqüência. Simulou-se de um modelo de circuito simples, com um transmissor e um receptor. Os resultados apresentados mostram a viabilidade técnica do projeto, sendo proposto para trabalhos futuros a implementação de um protótipo do transdutor eletrônico do tomógrafo capacitivo elétrico aplicado ao estudo do processo de adsorção.

Introdução: A comprovação da eficiência de formulações hidratantes deve ser criteriosa e analisada com métodos adequados. Objetivo: O objetivo principal do trabalho foi avaliar in vivo a eficácia hidratante de formulações contendo diferentes componentes ativos por capacitância elétrica e perda de água transepidérmica. Compararam-se os desempenhos entre Corneometer® e Moisturemeter® e entre o Vapometer® e Tewlmeter®. Verificou-se o comportamento in vitro das alterações causadas pelas substâncias hidratantes, em modelo de estrato córneo alternativo. Material e Métodos: Os compostos ativos selecionados (4% p/p) para incorporação nos géis à base de carbômero foram: uréia, extrato vegetal de Imperata cylindrica; complexo contendo fatores de hidratação natural; e os derivados do açúcar, sacarídeo isomerato e a mistura de xilitilglicosídeo e anidroxilitilglicosídeo. A avaliação in vivo da eficácia hidratante teve o delineamento experimental baseado no projeto fatorial ANOVA three way. Os tempos estudados foram: após a aplicação e 30, 60, 120; 240 e 360 minutos. O estudo de estabilidade acelerada das formulações envolveu condições drásticas de armazenamento (temperatura, umidade e luminosidade) durante 90 dias. Na avaliação in vitro do comportamento das substâncias hidratantes utilizou-se a espectroscopia Raman com transformada de Fourier (FT-Raman) e Calorimetria exploratória diferencial (DSC). Resultados: A análise estatística da capacitânia elétrica obtida por Corneometer® e do Moisturemeter® mostraram que houve diferenças significativas entre os géis e o tempo de aplicação. Com relação às medidas de perda de água transepidérmica, os resultados obtidos por Vapometer® e Tewlmeter® não apresentaram concordância. As bandas encontradas nos espectros FT-Raman mostraram que os ativos hidratantes não provocaram alterações na estrutura conformacional do estrato córneo alternativo. A análise da calorimetria (DSC) mostrou que o gel de uréia aumentou o conteúdo hídrico da membrana. Conclusão: Os géis contendo 4% (p/p) de uréia e de 4% (p/p) de derivado de açúcar apresentaram melhor eficácia hidratante in vivo, capacitância elétrica quando analisado por Corneometer® e Moisturemeter®. Em relação à perda de água transepidérmica, o gel base sem ativo obteve o melhor resultado. Com relação às medidas de capacitância, o Corneometer® e o Moisturemeter® mostraram-se estaticamente semelhantes. Comparando-se as medidas de perda de água transepidérmica, a análise estatística indicou que o Vapometer® tem precisão inferior comparada com o Tewlmeter®. A avaliação do comportamento in vitro das substâncias hidratantes sugeriram que as mesmas são seguras. / Introduction: Hydration of the corneal layer varies according to the amount of water present; the transportation of water from the lower layers; evaporation speed and quantity and composition of epicutaneous emulsion. Proof of moisturizer formula efficiency must be prudent and analyzed using appropriate methods. Objective: The studys main objective was to assess the in vivo efficacy of moisturizer formulas with different active components by means of electrical capacitance and transepidermal water loss. The accelerated stability of the referred to formulas was also observed and assessed. Performances between Corneometer® and Moisturemeter® and between Vapometer® and Tewlmeter® were compared. In vitro behavior of alterations caused by moisturizing substances was verified in an alternative corneal stratum model. Material and Methods: The active compounds selected (4% p/p) for use in carbomer-based gels were: urea, Imperata cylindrica vegetal extract; a complex with natural moisturizing factors; sugar byproducts, saccharide isomerate and the mix of xylitol glucoside and anhydro xylitol glicoside. In vivo assessment of moisturizing efficacy of the formulas by means of electrical capacitance and transepidermal water loss was designed based in ANOVA three way factorial design. The gels were applied on both arms of volunteers aged 20 to 30 and a control application (base gel) and an untreated area were used. Study times were: after application and at 30, 60, 120; 240 and 360 minutes. The accelerated stability study of the formulations involved drastic storage conditions (temperature, humidity, luminosity) over 90 days. For the in vitro assessment of moisturizing substance behavior, Raman spectroscopy was used with Fourier Transform (FT-Raman) and differential scanning calorimetry (DSC). Results: Statistical analysis of electrical capacitance using Corneometer® and Moisturemeter® revealed significant differences between the gels and application time. With regard to transepidermal water loss measures, the results obtained from Vapometer® and Tewlmeter® did not reveal concordance. The bands found in the FT-Raman spectrum revealed that the active moisturizers did not cause changes in the alternative cornea stratum conformation structure. Calorimetry (DSC) analysis showed the urea gel increased membrane water content. Conclusion: Gels containing 4% (p/p) urea and 4% (p/p) of sugar byproduct had the best in vivo moisturizing efficacy, electrical capacitance when analyzed with Corneometer® and Moisturemeter®. In relation to transepidermal water loss, the base gel without active ingredients had the best result in both Vapometer® and Tewlmeter®. The formulas were stable for a period of three months in the studied storage conditions. In relation to capacitance measures, Corneometer® and Moisturemeter® proved to be statistically similar. When comparing transepidermal water loss measures, statistical analysis indicated that Vapometer® is not as precise as Tewlmeter®. In vitro assessment of behavior of moisturizing substances suggested they are safe.

No description available.

The technological advancement in electrical machinery represents the need to understand the lubricant behaviour in the electrical environment. As shaft voltages are unavoidable in electrical machinery, developing new grease formulations and studying their performance against electric loads is required. The thesis aims to design, develop, install and validate a novel test machine to study grease performance under the influence of electric currents. The system aims to supply damaging electric currents through the bearing, but that was not possible to accomplish due to miscalculations. The test machine is designed to carry out experiments using angular contact bearings. The experiments were performed with four greases, Lithium-complex and polypropylene-based, of high and low base-oil viscosity, respectively. The study compares the frictional moments and self-induced temperatures in the bearings with and without the influence of electric currents. Along with the frictional moment measurements, the lubricant film thickness was estimated using the “electrical-capacitance” method to monitor the status of the lubricant inside the bearing in real-time. The test machine is limited to speeds up to 3600 rpm, and the project lays out a foundation for research in film thickness estimation in rolling element bearings. As a part of the thesis, new slip rings were specified to facilitate the test machine to perform studies at higher speeds up to (17000rpm). / De tekniska framstegen inom elektriska maskiner representerar behovet av att förstå smörjmedlets beteende i den elektriska miljön. Eftersom axelspänningar är oundvikliga i elektriska maskiner krävs utveckling av nya fettformuleringar och studier av deras prestanda mot elektriska belastningar. Avhandlingen syftar till att designa, utveckla, installera och validera en ny testmaskin för att studera fettprestanda under påverkan av elektriska strömmar. Systemet syftar till att leverera skadliga elektriska strömmar genom lagret, men det var inte möjligt att åstadkomma på grund av felberäkningar. Testmaskinen är designad för att utföra experiment med vinkelkontaktlager. Experimenten utfördes med fyra fetter, litiumkomplex- och polypropenbaserade, med hög respektive låg basoljeviskositet. Studien jämför friktionsmomenten och självinducerade temperaturer i lagren med och utan påverkan av elektriska strömmar. Tillsammans med mätningarna av friktionsmomentet uppskattades smörjmedelsfilmtjockleken med hjälp av metoden "elektrisk kapacitans" för att övervaka statusen för smörjmedlet inuti lagret i realtid. Testmaskinen är begränsad till hastigheter upp till 3600 rpm, och projektet lägger en grund för forskning inom filmtjockleksuppskattning i rullager. Som en del av avhandlingen specificerades nya släpringar för att underlätta för testmaskinen att utföra studier vid högre hastigheter upp till (17000rpm).

No description available.