Diss. (sammanfattning) Stockholm : Karol. inst., 2003. / Härtill 5 uppsatser.

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No. of bitstreams: 2 license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) Bruno_Regis_Lyrio_Ferraz.PDF: 3015137 bytes, checksum: d479e9335e2f200939b52075f9b84382 (MD5) Previous issue date: 2016 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Funda??o de Amparo a Pesquisa do Estado de Minas Gerais (FAPEMIG) / RESUMO Etionamida e pirazinamida s?o antibi?ticos ?teis no tratamento da tuberculose multirresistente. O presente trabalho descreve o desenvolvimento e valida??o de metodologias eletroanal?ticas para determina??o de etionamida e pirazinamida em formula??es farmac?uticas e em urina humana empregando um eletrodo de diamante dopado com boro e um eletrodo de carbono v?treo modificado comum filme de poli glicina. Durante o desenvolvimento de ambas as metodologias, a voltametria c?clica foi empregada para verificar a influ?ncia do pH, da velocidade de varredura e do eletr?lito suporte no comportamento eletroqu?mico de ambos os analitos, bem como foram calculados os n?meros de pr?tons e el?trons envolvidos em cada uma das rea??es eletroqu?micas. A voltametria de onda quadrada com os par?metros otimizados foi utilizada para construir curvas anal?ticas para a ETO e PZA. Para a ETO foi obtido um intervalo linear de 1,0 a 80,0 ?mol L?1, com LOD e LOQ iguais a 0,294 e 0,980 ?mol L?1, respectivamente. Para a PZA foi obtido um intervalo linear de 0,47 a 6,16 ?mol L?1, com LOD e LOQ iguais a 0,035 e 0,12 ?mol L?1, respectivamente. A precis?o foi avaliada pelo registro de voltamogramas no mesmo dia e em dias diferentes, obtendo-se desvios padr?es relativos, inferiores a 5,0% em ambos os m?todos. Os resultados dos estudos de interferentes mostraram que nenhuma das subst?ncias testadas interferiu de maneira significativa na determina??o de ambos os f?rmacos. Os m?todos desenvolvidos foram comparados estatisticamente com os protocolos oficiais da farmacopeia atrav?s do teste-t e do teste-F, e os resultados mostraram que os valores de t e F calculados foram menores do que os valores de t e F cr?ticos, indicando que n?o houve diferen?a estat?stica entre as m?dias. A exatid?o de ambos os m?todos foi avaliada tamb?m por estudos de adi??o e recupera??o, obtendo-se como resultados percentuais de recupera??o pr?ximos a 100% para ambos os m?todos. A valida??o das metodologias desenvolvidas foi realizada pela avalia??o dos par?metros anal?ticos como sensibilidade, seletividade, limite de detec??o, limite de quantifica??o, faixa linear, exatid?o e precis?o e os resultados obtidos foram satisfat?rios. Portanto, os m?todos desenvolvidos podem ser aplicados com sucesso na determina??o dos f?rmacos ETO e PZA em medicamentos e urina humana. / Disserta??o (Mestrado) ? Programa de P?s-gradua??o em Ci?ncias Farmac?uticas, Universidade Federal dos Vales do Jequitinhonha e Mucuri, 2016. / ABSTRACT Ethionamide and pyrazinamide antibiotics are useful in the treatment of multidrugresistant tuberculosis. This work describes the development and validation of electroanalytical methodologies for determination of ethionamide and pyrazinamide in pharmaceutical formulation and human urine using boron-doped diamond electrode and poly glycine modified glassy carbon electrode, respectively. During the development of both methodologies, cyclic voltammetry was used to investigate the influence of pH, scan rate and the supporting electrolyte on the electrochemical behavior of both analytes, as well as the numbers of protons and electrons involved in each of the electrochemical reactions were calculated. Square wave voltammetry with optimized parameters were used to construct standard curves for ETO and PZA. For ETO a linear range from 1.0 to 80.0 ?mol L?1 was obtained with LOD and LOQ equal to 0.294 and 0.980 ?mol L?1, respectively. For PZA a linear range from 0.47 to 6.16 ?mol L?1was obtained with LOD and LOQ equal to 0.035 and 0.12 ?mol L?1, respectively. The precision was evaluated by voltammograms record on the same day and on different days, obtaining relative standard deviation less than 5.0% in both methods. The results of interfering studies showed that none of the tested substance interferes significantly in the determination of both drugs. The developed methods were statistically compared with the pharmacopoeia official protocols through the t-test and F-test, and the results showed that the calculated t and F values were lower than the critical t and F values indicating that there was no statistical difference between the averages. The accuracy of both methods was also evaluated by addition and recovery studies, obtaining results as percentage recovery close to 100% for both methods. The validation of the developed methodologies was carried out by the evaluation of analytical parameters such as sensitivity, selectivity, detection limit, quantification limit, linear range, accuracy and precision and the obtained results were satisfactory. Therefore, the developed methods can be applied successfully in the determination of ETO and PZA drugs in pharmaceuticals and human urine.

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No. of bitstreams: 1 santos_jc_dr_guara.pdf: 78449557 bytes, checksum: 4515b9cb7cc346753f7e9682b8e037de (MD5) Previous issue date: 2018-07-04 / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / Nowadays, despite the technological development experienced by science in general, a fact especially evident by the available powerful computer machines, the analytical and semi-analytical methods to study different space problems are still of great importance in the fields of astrodynamics and celestial mechanics. From the physical understanding of the motion of celestial bodies to the planing and designing of space missions, the use of mathematical models to deal with a very large number of contemporary problems plays a fundamental role in the progress of human knowledge. In this context, the present thesis presents the use of different mathematical techniques to deal with different various and current problems in astrodynamics and celestial mechanics. The studies developed throughout this work are applicable to both areas. The topics studied are the following ones: (1) The development of disturbing potentials using the double-averaging process, in order to be included in the Lagrange planetary which are numerically integrated to study features of orbits around Mercury and the Galilean moon Callisto; (2) The use of different perturbation integrals, techniques to identify and map different perturbations present in a planetary system, with focus on the analysis of systems of Giant planets with their massive moons; (3) The use of the concept of intermediary Hamiltonian and the use of a canonical transformation called elimination of the parallax, both to deal with binary systems in the context of the roto-orbital dynamics, this one as an approach of the fulltwo body problem; (4) An updated analysis of Gauss variational equations to study quasisatellite orbits around the Martian moon Phobos and with analytical predictions made after obtaining linear and averaged equations of motions. Therefore, this thesis intend not only to provide important analysis and results for each specific problem which it deals with along its pages, but also seeks to highlighting the merit and current relevance of different analytical and semi-analytical methods to be used in the fields of astrodynamics and celestial mechanics. Additionally, the author also hopes to offer an outcome of diverse interesting ideas and methods to be explored in future investigations in these research fields / Na atualidade, a despeito do desenvolvimento tecnológico experimentado pela ciência em geral, algo especialmente evidenciado por poderosas máquinas computacionais disponíveis, os métodos analíticos e semianalíticos para o estudo de diferentes problemas espaciais ainda são de grande importância nos campos de astrodinâmica e mecânica celeste. Desde a compreensão física do movimento de corpos celestes até ao planejamento e projeto de missões espaciais, o uso de modelos matemáticos para lidar com um grande número de problemas contemporâneos desempenha um papel fundamental no progresso do conhecimento humano. Neste contexto, a presente tese apresenta o uso de diferentes técnicas matemáticas para lidar com diversos e atuais problemas em astrodinâmica e mecânica celeste. Os estudos desenvolvidos ao longo deste trabalho são aplicáveis à ambas as áreas. Os tópicos estudados são os seguintes: (1) O desenvolvimento de potenciais perturbadores usando o processo de dupla média, de forma a serem incluídos nas equações planetárias de Lagrange que são integradas numericamente para estudar características de órbitas ao redor de Mercúrio e da lua galileana Calisto; (2) A utilização de diferentes integrais de perturbação, técnicas para identificar e mapear diferentes perturbações presentes em um sistema planetário, com foco na análise de sistemas de planetas gigantes com suas luas massivas; (3) A utilização do conceito de hamiltoniana intermediária e o uso de uma transformação canônica chamada eliminação da paralaxe, ambos para lidar com sistemas binários no contexto da dinâmica roto-orbital, essa sendo uma aproximação do problema completo de dois corpos; (3) Uma análise atualizada de equações variacionais de Gauss para o estudo de órbitas quasi-satélite ao redor da lua marciana Fobos e com predições analíticas realizadas após serem obtidas equações de movimento linearizadas e com média. Portanto, esta tese pretende não somente prover importantes análises e resultados para cada problema específico com os quais a mesma lida ao longo de suas páginas, mas também procura destacar o mérito e relevância atual de diferentes métodos analíticos e semianalíticos a serem utilizados nos campos de astrodinâmica e mecânica celeste. Adicionalmente, o autor também espera oferecer um produto de variadas ideias e métodos a serem explorados em futuras investigações nesses campos de pesquisa / 2013/26652-4 / 2015/18881-9

Perante diversas situações da engenharia são utilizadas formulações empíricas de dimensionamento baseadas em dados de campo e experiência profissional que definem muito o caráter subjetivo da metodologia padrão de projeto. O presente trabalho de pesquisa aborda os diversos métodos de obtenção dos esforços gerados em dutos enterrados submetidos a cargas dinâmicas e estáticas e sua posterior reavaliação através de modelagem numérica com o programa Plaxis 3D. Os métodos analíticos não convencionais foram comparados com o método padrão de cálculo sendo que o mesmo demonstrou ter uma boa precisão mesmo sem considerar outros fatores importantes como a parcela de resistência devida à coesão do solo e sua deformabilidade. A modelagem numérica demonstrou o conservadorismo do método de Marston e o subdmensionamento do espraiamento em prisma devido aos efeitos locais ocasionados pela adoção do recobrimento mínimo e sobrecarga dinâmica elevada. Também se observou, através da modelagem 3D, que a utilização dos dois métodos clássicos favorecem a obtenção de resultados dentro da razoabilidade.Verificou-se também, como resultado desta pesquisa, que a proposta de um método clássico modificado permite uma melhor aproximação da carga que atinge o duto. / In various engineering situations, empirical formulations of design, based on field data and professional experience which highly define the subjective nature of the standard design methodology, are used. This paper discusses the various methods of obtaining the stresses generated in buried pipelines, which are subjected to static and dynamic loads, and their subsequent re-evaluation by numerical modeling with Plaxis 3D program. The non-conventional analytical methods were compared with the standard method of calculation and it has demonstrated good accuracy even without considering other factors such as soil cohesion and deformability. The numerical modeling demonstrated the conservatism of the Marston method and subsiding of the prism spread due to local effects caused by the adoption of minimum cover and high dynamic overload and due to how the use of two classical methods favor reasonable results. A classic modified method that would allow a closer approximation of the load was also proposed.

[pt] A análise de sistemas de medição consiste do exame da adequação do sistema quanto ao operador, ao instrumento e a outras fontes de variação, bem como da comparação da variância do erro de medição com a variância natural do processo. Nesse aspecto, esta pesquisa teve por objetivo a análise das incertezas da quantificação de fase pelo método de Rietveld em análise de pó. Os efeitos de vários fatores na quantificação de fase foram avaliados utilizando técnicas estatísticas de planejamento experimental e de análise multivariada, com a utilização de materiais de alto nível de rastreabilidade na realização dos experimentos, no Laboratório de difração de raios X do Departamento de Ciências de Materiais e Metalurgia da PUC-Rio. Através da determinação do construto de variação do processo, constatou-se que a quantificação das fases analisadas sofre influência das condições de medição de forma diferenciada de material para material, impossibilitando a obtenção de uma fórmula geral para cálculo dos erros de quantificação, embora os erros possam ser determinados por uma análise de repetitividade e reprodutibilidade apropriadamente conduzida. / [en] The analysis of measurement systems is done by the examination of the adequacy of the system according to the operator, the instrument and other sources of variability, as well as by the comparison of the measurement error variance with the natural process variance. This research consisted in the evaluation of the uncertainties of phase quantification in powder analysis by the Rietveld method. The evaluation of the effects of several factors on the phase quantification was performed using statistical techniques of design of experiments and of multivariate analysis, with the use of materials of high level of traceability for the conduction of the experiments, in the Laboratory of X-ray Diffraction of the Pontifícia Universidade Católica do Rio de Janeiro. Through the determination of the variational structure of the process it was verified that the analyzed phases suffer influence of the measurement conditions in a differentiated way, which prevents the obtention of a general formula for calculation of the quantification error, although the errors can be determined by a repeatability and reproducibility analysis properly conducted.

Perante diversas situações da engenharia são utilizadas formulações empíricas de dimensionamento baseadas em dados de campo e experiência profissional que definem muito o caráter subjetivo da metodologia padrão de projeto. O presente trabalho de pesquisa aborda os diversos métodos de obtenção dos esforços gerados em dutos enterrados submetidos a cargas dinâmicas e estáticas e sua posterior reavaliação através de modelagem numérica com o programa Plaxis 3D. Os métodos analíticos não convencionais foram comparados com o método padrão de cálculo sendo que o mesmo demonstrou ter uma boa precisão mesmo sem considerar outros fatores importantes como a parcela de resistência devida à coesão do solo e sua deformabilidade. A modelagem numérica demonstrou o conservadorismo do método de Marston e o subdmensionamento do espraiamento em prisma devido aos efeitos locais ocasionados pela adoção do recobrimento mínimo e sobrecarga dinâmica elevada. Também se observou, através da modelagem 3D, que a utilização dos dois métodos clássicos favorecem a obtenção de resultados dentro da razoabilidade.Verificou-se também, como resultado desta pesquisa, que a proposta de um método clássico modificado permite uma melhor aproximação da carga que atinge o duto. / In various engineering situations, empirical formulations of design, based on field data and professional experience which highly define the subjective nature of the standard design methodology, are used. This paper discusses the various methods of obtaining the stresses generated in buried pipelines, which are subjected to static and dynamic loads, and their subsequent re-evaluation by numerical modeling with Plaxis 3D program. The non-conventional analytical methods were compared with the standard method of calculation and it has demonstrated good accuracy even without considering other factors such as soil cohesion and deformability. The numerical modeling demonstrated the conservatism of the Marston method and subsiding of the prism spread due to local effects caused by the adoption of minimum cover and high dynamic overload and due to how the use of two classical methods favor reasonable results. A classic modified method that would allow a closer approximation of the load was also proposed.

This master´s thesis is focused on analysis of the company which is situated in the pro-duction of plastic windows and profile systems. Analysis of the actual state is made through the analysis of the inner and outer environment, financial situaction is estimated with the Kralicek Quick Test. Thesis includes suggestions and recommendations which will cause improvement of the situation at general in following years.

Under produktionen av kartong vid det integrerade massa- och kartongbruket, som ägs av Holmen Iggesund Paperboard AB, bildas klorat som är giftigt för vattenlevande organismer. Därför är det väsentligt att utsläppet av klorat till havet, via avloppsvattnet från bruket, hålls under de gränsvärden som fastställts. För att övervaka kloratutsläppet analyseras prover på avloppsvattnet rutinmässigt, och en jonkromatograf ämnades tas i drift för ändamålet. Jonkromatografi är en standardiserad metod för analys av klorat, som måste verifieras innan den tas i bruk. Inga explicita krav fanns på hur omfattande verifieringen skulle vara. Ett syfte med studien var därför att utveckla generella rekommendationer för omfattningen av verifieringen av en standardiserad analysmetod. Litteratur angående verifiering eftersöktes och summerades, och utifrån den togs en verifieringsplan för jonkromatografisk analys av klorat fram. Mätresultat som erhölls utvärderades statistiskt. Slutsatserna var; att verifiering bör planeras på ett sätt så att kalibrering och underhåll av instrumentet sker i samma omfattning som är tänkt vid rutinanvändning av analysmetoden; selektivitet bör testas tidigt, och riktiga prover bör analyseras i ett tidigt skede; omfattningen av verifieringen med avseende på provmatriser och koncentrationsnivåer ska återspegla de provmatriser och koncentrationer som analysmetoden kommer att innefatta i rutinarbetet; antalet försök som bör inkluderas beror på kraven som ställs på de olika egenskaper som definierar prestandan. Minst 6 försök på varje provmaterial var ett riktmärke för precision och riktighet, medan ett försök räckte vid utvärdering av selektivitet och instrumentets mätområde. För att kunna säkerställa god analyskvalité, är utbildning i analysmetodik en viktig del. Ytterligare ett syfte med denna studie var att undersöka utbildningsverksamhetens lärandemål, samt vilka utmaningar som fanns inom utbildningen i analysmetodik. Genom fokusgruppintervjuer och observationer samlades information inom utbildningsverksamheten och dess utmaningar. Utifrån det teoretiska ramverket självstyrd inlärning utfördes en deduktiv tematisk analys av den insamlade datan. Slutsatserna av arbetet löd: Det övergripande syftet med upplärningen inom en analysmetod var att personen som genomgått utbildningen ska kunna ansvara för att tillämpa analysmetoden självständigt utifrån instruktionen, ha kunskap om rimliga mätresultat, kunna reflektera över sitt arbete, samt ha kunskap om syftet med analysmetoden. Ingen standardiserad mall för vad som ska ingå i utbildningen inom en analysmetod fanns, vilket bidrog till osäkerheter angående huruvida likvärdig kompetens uppnåddes för personer under utbildning; dagens utbildningsupplägg inbjöd inte till att personen under upplärning tog på sig ansvaret för uppfyllandet av lärandemålen i den utsträckning som önskades. För att möjliggöra detta föreslogs att ett förberedande moment skulle införas, samt att den lärande skulle få mer tid och möjlighet att genomföra delar av utbildningen självständigt. / During the production of paperboard at the integrated pulp and paperboard mill, owned by Holmen Iggesund Paperboard AB, chlorate is formed, which is a toxic compound for aquatic organisms. It is therefore essential that the chlorate levels in the wastewater from the mill, which is released to the ocean, are below the established limit. In order to monitor the effluent of chlorate, wastewater samples are routinely analyzed, and for this purpose an ion chromatograph was intended to be put to use. Ion chromatography is a standardized method for chlorate analysis, which needs to be verified before being used for routine analyses. No explicit requirements regarding the extent of the verification existed. One purpose of this study was therefore to develop general recommendations regarding the extent of verification of a standardized analytical method. Literature regarding verification was sought for and summarized. Based on the literature, a plan for verifying ion chromatographic analysis of chlorate was constructed. The measurement results obtained were evaluated statistically. Conclusions drawn were: calibration and maintenance of the instrument during the verification process should reflect the frequency of maintenance and calibration planned during the routine use; selectivity should be tested early on, as well as real samples; the extent of the verification with respect to matrices and concentration levels should reflect those that will be included in the routine use of the analytical method; the number of experiments included depends on the requirements imposed on the performance characteristics of the method. At least 6 experiments for each sample was a good aim for verifying precision and trueness, while one experiment was enough for verification of selectivity and the working range of the instrument. In order to ensure satisfactory analysis quality, training in analytical methods is an important aspect. Another purpose of this study was to investigate the learning objectives of the educational activities as well as what challenges could be identified with respect to training in analytical methods. Through focus group interviews and observations, data was collected about the educational activities and challenges. Based on the theoretical framework self-directed learning, a deductive thematic analysis was performed. Conclusions were: The overall purpose of the training in analytical methods was that the person who underwent training should be able to independently apply the analytic method, with the aid of the analytical instruction, have the necessary knowledge about reasonable results, be able to reflect about their work and have knowledge about the purpose of the analytical method. No standardized template regarding what should be included in the training existed, which contributed to uncertainties regarding if equivalent knowledge was achieved for persons under training. The educational approach of today did not encourage the person under training enough to take responsibility for fulfilling the learning objectives. To enable this, it was suggested that a preparation element should be included in the training, and also that the person under training should get more time and opportunities to complete some of the training independently.

Recombination mechanisms in gallium arsenide have been studied using temperature-dependent time-resolved photoluminescence-decay. New analytical methods are presented to improve the accuracy in bulk lifetime measurement, and these have been used to resolve the temperature-dependent lifetime. Fits to temperature-dependent lifetime yield measurement of the radiative-efficiency, revealing that samples grown by the Czochralski and molecular-beam-epitaxy methods are limited by radiative-recombination at 77K, with defect-mediated nonradiative-recombination becoming competitive at 300K and above. In samples grown with both doping types using molecular-beam-epitaxy, a common exponential increase in capture cross-section characterized by a high value of E_infinity=(258 +/- 1)meV was observed from the high-level injection lifetime over a wide temperature range (300-700K). This common signature was also observed from 500-600K in the hole-lifetime observed in n-type Czochralski GaAs where E_infinity=(261 +/- 7)meV was measured, which indicates that this signature parametrizes the exponential increase in hole-capture cross-section. The high E_infinity value rules out all candidate defects except for EL2, by comparison with hole-capture cross-section data previously measured by others using deep-level transient spectroscopy. / Thesis / Doctor of Philosophy (PhD)

Объектами исследования служили фармацевтическая субстанция «Аргамид» и готовая лекарственная форма 1% крем «Аргамид» на основе серебряной соли сульфадимидина (Приоритетная справка на выдачу патента № 2015153574 от 14.12.2015). Данная соль и лекарственные средства на ее основе были разработаны на базе кафедры фармации УГМУ с целью обеспечения российского фармацевтического рынка эффективными антибактериальными и ранозаживляющими лекарственными препаратами отечественного производства согласно стратегии развития фармацевтической промышленности «ФАРМА-2020». Цель работы: разработка и валидация методик количественного определения серебра в исследуемых лекарственных средствах. Анализ литературных данных показал, что оптимальным методом определения серебра является метод осадительного титрования с потенциометрической индикацией конечной точки титрования. При этом, учитывая содержание серебра в анализируемых лекарственных средствах, для его определения в субстанции был выбран метод роданометрического, а в готовой лекарственной форме – йодометрического титрования. Для анализируемых лекарственных средств были подобраны оптимальные условия пробоподготовки: масса навески, концентрация растворителя; время и температура обработки пробы. В качестве индикаторного вместо дорогостоящего импортного серебряного дискового электрода использовали отечественный толстопленочный серебросодержащий электрод. Положительные результаты валидационной оценки разработанных методик, проведенной согласно требованиям Государственной Фармакопеи РФ XIII изд., позволяют считать их приемлемыми и рекомендовать для включения в проекты фармакопейных статей на исследуемые лекарственные средства. Контроль содержания серебра по разработанным методикам не требует дорогостоящего оборудования, привлечения высококвалифицированного персонала, отличается относительно коротким временем анализа, а, следовательно, может применяться испытательными лабораториями предприятия в процессе производства и центрами контроля качества во время обращения на фармацевтическом рынке исследуемых лекарственных средств. / The objects of study were pharmaceutical substance "Argamid" and finished dosage form of 1% cream "Argamid" based on silver salt sulfadimidine (Priority reference patent number 2015153574 from 14.12.2015). This salt and drugs based on it have been developed at the Department of Pharmacy UGMU to ensure that the Russian pharmaceutical market effective antibacterial and wound healing medicines domestic production according to the strategy of development of the pharmaceutical industry "Pharma 2020". Objective: Development and validation of methods of quantitative determination of silver in the investigational medicinal product. Analysis of published data shows that the best method of determining silver is the method of precipitation titration with potentiometric indication end point. However, given the content of silver in the analyzed medicaments for identification substance rodanometricheskogo method was selected, and in the final dosage form - iodometric titration. optimal conditions for sample preparation were selected to be analyzed drugs: sample weight, the concentration of solvent; Sample processing time and temperature. As an indicator instead of expensive imported silver disk electrode used domestic thick-film silver-electrode. Positive results validation assessment developed techniques conducted in accordance with the requirements of the RF State Pharmacopoeia XIII ed., Allow us to consider them acceptable and recommended for inclusion in the draft articles on the pharmacopoeia investigational medicinal products. Control of the silver content by developed techniques does not require expensive equipment, highly skilled personnel, has a relatively short analysis time, and, therefore, can be applied testing laboratories of the enterprise in the production process and quality control center during handling in the pharmaceutical market of investigational medicinal products.