Determinação do teor de diclofenaco sódico em comprimidos por espectroscopia no infravermelho próximo NIR com calibração multivariada PLS

This work is combined with the potential of the technique of near infrared spectroscopy - NIR and chemometrics order to determine the content of diclofenac tablets, without destruction of the sample, to which was used as the reference method, ultraviolet spectroscopy, which is one of the official methods. In the construction of multivariate calibration models has been studied several types of pre-processing of NIR spectral data, such as scatter correction, first derivative. The regression method used in the construction of calibration models is the PLS (partial least squares) using NIR spectroscopic data of a set of 90 tablets were divided into two sets (calibration and prediction). 54 were used in the calibration samples and the prediction was used 36, since the calibration method used was crossvalidation method (full cross-validation) that eliminates the need for a validation set. The evaluation of the models was done by observing the values of correlation coefficient R 2 and RMSEC mean square error (calibration error) and RMSEP (forecast error). As the forecast values estimated for the remaining 36 samples, which the results were consistent with the values obtained by UV spectroscopy

Membranas fluorescentes para fototerapia regenerativa: produção e caracterização

Dissertação para obtenção do Grau de Mestre em Engenharia Biomédica

Caracterização de substâncias húmicas extraídas de solos e de lodo orgânico

No presente trabalho, foi estudada a extração de substâncias húmicas (SH) de horizontes A de dois solos do Rio Grande do Sul (Latossolo Roxo (LR), e Brunizém vértico (B)) e de um lodo orgânico (LO), oriundo da fabricação de celulose, empregando-se dois métodos: (1) as SH foram extraídas com solução de NaOH 0,5 mol L-1, após tratamento prévio com HCl 0,5 mol L-1; (2) foi introduzida a extração com solução de pirofosfato de sódio 0,15 mol L-1 (pH 7) antes da etapa alcalina. Em cada etapa, os teores de SH, de ácidos fúlvicos (AF) e de ácidos húmicos (AH) foram determinados por métodos espectroscópicos e gravimétricos e, no método 2, os teores de Fe, Al, Si e Ca foram medidos nos extratos por absorção atômica. A composição elementar de ácidos húmicos foi determinada, e sua estrutura e características químicas foram avaliadas a partir de razões C/N, (atômicas) H/C e O/C e a partir de dados de espectroscopia Ultravioleta/Visível (UV/Vis). No LR, o método 1 extraiu maior quantidade de SH, enquanto, no método 2, a etapa com pirofosfato extraiu apenas AF. Em contrapartida, no solo B, o método 2 foi mais eficiente, verificando-se maior rendimento na etapa com pirofosfato. A partir desses resultados, infere-se que as SH, no LR, interagem principalmente por meio de reação de trocas de ligantes e de pontes de hidrogênio e, no solo B, a interação por meio de pontes de cátions é um mecanismo importante. Os AH extraídos com NaOH apresentaram valores mais elevados para a razão H/C e valores inferiores para a razão O/C do que os extraídos com pirofosfato, indicando que o extrator neutro solubilizou SH de caráter aromático e grau de oxigenação superiores.

Obtenção e caracterização de compósitos de borracha natural e polianilina com ferrita de bário

Pós-graduação em Ciência dos Materiais - FEIS

Filmes finos obtidos a plasma em reagentes contendo ácido cítrico/etilenoglicol

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Caracterização estrutural e propriedades óticas e mecânicas do diglime polimerizado a plasma

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Determination of degree of ionization of poly(allylamine hydrochloride) (PAH) and poly[1-[4-(3-carboxy‑4 hydroxyphenylazo)benzene sulfonamido]-1,2-ethanediyl, sodium salt] (PAZO) in layer-by-layer films using vacuum photoabsorption spectroscopy

Electrostatic and hydrophobic interactions govern most of the properties of supramolecular systems, which is the reason determining the degree of ionization of macromolecules has become crucial for many applications. In this paper, we show that highresolution ultraviolet spectroscopy (VUV) can be used to determine the degree of ionization and its effect on the electronic excitation energies of layer-by-layer (LbL) films of poly(allylamine hydrochloride) (PAH) and poly[1-[4-(3-carboxy-4 hydroxyphenylazo)- benzene sulfonamido]-1,2-ethanediyl, sodium salt] (PAZO). A full assignment of the VUV peaks of these polyelectrolytes in solution and in cast or LbL films could be made, with their pH dependence allowing us to determine the p'K IND. a' using the Henderson-Hasselbach equation. The p'K IND. a' for PAZO increased from ca. 6 in solution to ca. 7.3 in LbL films owing to the charge transfer from PAH. Significantly, even using solutions at a fixed pH for PAH, the amount adsorbed on the LbL films still varied with the pH of the PAZO solutions due to these molecular-level interactions. Therefore, the procedure based on a comparison of VUV spectra from solutions and films obtained under distinct conditions is useful to determine the degree of dissociation of macromolecules, in addition to permitting interrogation of interface effects in multilayer films.

Antibacterial activity of the marine sponge Ircinia Campana collected at Punta Uva Limón against Staphylococcus Aureus

The sponges are simple multicellularorganisms; they inhabit in marine environments from the polar seas to the tropical waterswhere they are more abundant. These species are exposed to large populations of microbes, reason that explains their complex morphological and cellular defense mechanism, which are used by these organisms to fight against pathogens. The purpose of this study was to evaluate the antibacterial activity of the marine sponge Ircinia campana, whichinhabits in the south of the Caribbean coast of Costa Rica against  Sthapylococcus aureus gram-positive bacteria. Sampleswere collected in Punta Uva in Limónduring July of 2007. The active compounds were obtainedby extraction with acetone (crude extract); and subsequently, chromatographic extracts were obtained using fractions 1:4 hexane: ethyl acetate. The antibacterial activities of the different fractions, including the  crude extract were tested.Our results suggest a zone of inhibition of 14.60 ±0.25 mm for the crude extract and18.70±0.25mm for the most active fraction separated by chromatography. The metabolite responsible for the antibacterial activity was isolated by High Performance Liquid Chromatography (HPLC)and preliminarily characterized through ultraviolet (UV) and infrared (IR) spectroscopy.

Remoción de la hemoglobina por adsorción sobre nanopartículas magnéticas de Fe3O4/TiO2

La remoción de la hemoglobina (Hb) por adsorción de la proteína sobre nanopartículas (Nps) magnéticas de Fe3O4/TiO2 (núcleo/coraza) aplicando un campo magnético externo, fue investigada mediante espectroscopia ultravioleta en el rango del ultravioleta y visible (UV-VIS). Durante la etapa de contacto de las Nps con la Hb se varió la concentración de las Nps y la temperatura, complementariamente durante la etapa de remoción del complejo Fe3O4/TiO2-Hb se varió la intensidad del campo magnético externo. Con una concentración inicial de Nps de 8 mg ml-1, el valor de la absorbancia del sobrenadante disminuye en un 11% con respecto a la solución inicial de Hb (0,8 g l-1) y al aumentar en un 50% la concentración de Nps, el valor disminuye hasta un 17%. Al incrementar la temperatura de 25 a 35ºC disminuye la adsorción de la Hb pero no se observa indicios de desnaturalización de la misma. Durante la etapa de remoción del complejo Fe3O4/TiO2-Hb, al incrementar la fuerza magnética se logra una caída en la intensidad de la absorbancia, casi un 30%. Finalmente, se determinó la demanda bioquímica de oxígeno (DBO5) de la solución inicial de Hb y del sobrenandante, el valor para la solución inicial de Hb fue de 100 mg ml-1 y los resultados obtenidos para todas las soluciones tratadas fueron inferiores (62 mg ml-1) verificando el impacto que tuvo el uso de las Nps magnéticas de Fe3O4/TiO2 en la remoción de la Hb.

Design of functional hybrid coatings with anti-biofouling, self-cleaning and anti-reflecting applications

263 p.

Modelo de calibração da concentração de metilmetacrilato em solução aquosa utilizando espectroscopia de absorção no ultravioleta

Dilutions of methylmetacrylate ranging between 1 and 50 ppm were obtained from a stock solution of 1 ml of monomer in 100 ml of deionised water, and were analyzed by an absorption spectrophotometer in the UV-visible. Absorbance values were used to develop a calibration model based on the PLS, with the aim to determine new sample concentrations. The number of latent variables used was 6, with the standard errors of calibration and prediction found to be 0,048 ml/100 ml and 0,058 ml/100 ml. The calibration model was successfully used to calculate the concentration of monomer released in water, where complete dentures were kept for one hour after polymerization.

Estabilidade de cor de resinas compostas em função de composição e sistema de fotoativação: avaliação através de espectroscopia de reflectância

Pós-graduação em Ciências Odontológicas - FOAR

Caracterização por espectroscopia vibracional de filmes Layer-by-Layer contendo ftalocianina, polímeros condutores e gomas naturais

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Potenciais periódicos: aplicação à espectroscopia do benzeno

Pós-graduação em Física - FEG

Interconexión monolítica de dispositivos fotovoltaicos basados en a-Si mediante ablación directa con fuentes láser ultravioleta

Resumen En la última década la tecnología láser se ha convertido en una herramienta imprescindible en la fabricación de dispositivos fotovoltaicos, muy especial¬mente en aquellos basados en tecnología de lámina delgada. Independiente¬mente de crisis coyunturales en el sector, la evolución en los próximos años de estas tecnologías seguirá aprovechándose de la flexibilidad y calidad de proceso de la herramienta láser para la consecución de los dos objetivos básicos que harán de la fotovoltaica una opción energética económicamente viable: la reducción de costes de fabricación y el aumento de eficiencia de los dispositivos. Dentro de las tecnologías fotovoltaicas de lámina delgada, la tecnología de dispositivos basados en silicio amorfo ha tenido un gran desarrollo en sistemas estándar en configuración de superestrato, pero su limitada efi¬ciencia hace que su supervivencia futura pase por el desarrollo de formatos en configuración de substrato sobre materiales flexibles de bajo coste. En esta aproximación, las soluciones industriales basadas en láser actualmente disponibles para la interconexión monolítica de dispositivos no son aplica¬bles, y desde hace años se viene investigando en la búsqueda de soluciones apropiadas para el desarrollo de dichos procesos de interconexión de forma que sean transferibles a la industria. En este contexto, esta Tesis propone una aproximación completamente orig¬inal, demostrando la posibilidad de ejecutar una interconexión completa de estos dispositivos irradiando por el lado de la lámina (es decir de forma com¬patible con la opción de configuración de substrato y, valga la redundancia, con el substrato del dispositivo opaco), y con fuentes láser emitiendo en UV. Este resultado, obtenido por primera vez a nivel internacional con este trabajo, aporta un conocimiento revelador del verdadero potencial de estas fuentes en el desarrollo industrial futuro de estas tecnologías. Si bien muy posiblemente la solución industrial final requiera de una solución mixta con el empleo de fuentes en UV y, posiblemente, en otras longitudes de onda, esta Tesis y su planteamiento novedoso aportan un conocimiento de gran valor a la comunidad internacional por la originalidad del planteamiento seguido, los resultados parciales encontrados en su desarrollo (un número importante de los cuales han aparecido en revistas del JCR que recogen en la actualidad un número muy significativo de citas) y porque saca además a la luz, con las consideraciones físicas pertinentes, las limitaciones intrínsecas que el desarrollo de procesos de ablación directa selectiva con láseres UV en parte de los materiales utilizados presenta en el rango temporal de in¬teracción de ns y ps. En este trabajo se han desarrollado y optimizado los tres pasos estándar de interconexión (los habitualmente denominados Pl, P2 y P3 en la industria fotovoltaica) demostrando las ventajas y limitaciones del uso de fuentes en UV tanto con ancho temporal de ns como de ps. En particular destaca, por el éxito en los resultados obtenidos, el estudio de procesos de ablación selectiva de óxidos conductores transparentes (en este trabajo utilizados tanto como contacto frontal así como posterior en los módulos) que ha generado resultados, de excelente acogida científica a nivel internacional, cuya aplicación trasciende el ámbito de las tecnologías de silicio amorfo en lámina delgada. Además en este trabajo de Tesis, en el desarrollo del objetivo citado, se han puesto a punto técnicas de análisis de los procesos láser, basadas en métodos avanzados de caracterización de materiales (como el uso combi¬nado de la espectroscopia dispersiva de rayos X y la microscopía confocal de barrido) que se presentan como auténticos avances en el desarrollo de técnicas específicas de caracterización para el estudio de los procesos con láser de ablación selectiva de materiales en lámina delgada, procesos que no solo tienen impacto en el ámbito de la fotovoltaica, sino también en la microelectrónica, la biotecnología, la microfabricación, etc. Como resultado adicional, parte de los resultados de este trabajo, han sido aplicados exi¬tosamente por el grupo de investigaci´on en la que la autora desarrolla su labor para conseguir desarrollar procesos de enorme inter´es en otras tec-nolog´ıas fotovoltaicas, como las tecnolog´ıas est´andar de silicio amorfo sobre vidrio en configuraci´on de superestrato o el procesado de capas delgadas en tecnolog´ıas convencionales de silicio cristalino. Por u´ltimo decir que este trabajo ha sido posible por una colaboraci´on muy estrecha entre el Centro L´aser de la UPM, en el que la autora de¬sarrolla su labor, y el Grupo de Silicio Depositado del Centro de Inves¬tigaciones Energ´eticas, Medioambientales y Tecnol´ogicas, CIEMAT, que, junto al Grupo de Energ´ıa Fotovoltaica de la Universidad de Barcelona, han preparado la mayor parte de las muestras utilizadas en este estudio. Dichas colaboraciones se han desarrollado en el marco de varios proyectos de investigaci´on aplicada con subvenci´on pu´blica, tales como el proyecto singular estrat´egico PSE-MICROSIL08 (PSE-120000-2006-6), el proyecto INNDISOL (IPT-420000-2010-6), ambos financiados porel Fondo Europeo de Desarrollo Regional FEDER (UE) ”Una manera de hacer Europa y el MICINN, y los proyectos de Plan Nacional AMIC (ENE2010-21384-C04-´ 02) y CLASICO (ENE2007-6772-C04-04), cuya financiaci´on ha permitido en gran parte llevar a t´ermino este trabajo Abstract In the last decade, the laser technology has turned into an indispensable tool in the production of photovoltaic devices, especially of those based on thin film technology. Regardless the current crisis in the sector, the evolution of these technologies in the upcoming years will keep taking advantage of the flexibility and process quality of the laser tool for the accomplishment of the two basic goals that will convert the photovoltaic energy into economically viable: the manufacture cost reduction and the increase in the efficiency of the devices. Amongst the thin film laser technologies, the technology of devices based on amorphous silicon has had a great development in standard systems of superstrate configuration, but its limited efficiency makes its survival de¬pendant on the development of formats in substrate configuration with low cost flexible materials. In this approach, the laser industrial solutions cur¬rently available for the monolithic interconnection are not applicable, and in the last few years the investigations have been focused on the search of appropriate solutions for the development of such interconnection processes in a way that the same are transferable to the industry. In this context, this Thesis proposes a totally original approach, proving the possibility of executing a full interconnection of these devices by means of irradiation from the film side, i.e., compatible with the substrate con¬figuration, and with UV laser sources. This result, obtained for the first time at international level in this work, provides a revealing knowledge of the true potential of these sources in the future industrial development of these technologies. Even though very probably the final industrial solution will require a combination of the use of UV sources along with other wave¬lengths, this Thesis and its novel approach contribute with a high value to the international community because of the originality of the approach, the partial results found throughout its development (out of which, a large number has appeared in JCR journals that currently accumulate a signifi¬cant number of citations) and brings to light, with the pertinent scientific considerations, the intrinsic limitations that the selective direct ablation processes with UV laser present in the temporal range of interaction of ns and ps for part of the materials used in this study. More particularly, the three standard steps of interconnection (usually de¬nominated P1, P2 and P3 in the photovoltaic industry) have been developed and optimized, showing the advantages as well as the limitations of the use of UV sources in both the ns and ps pulse-width ranges. It is highly remark¬able, because of the success in the obtained results, the study of selective ablation processes in transparent conductive oxide (in this work used as a front and back contact), that has generated results, of excellent interna¬tional scientific reception, whose applications go beyond the scope of thin film photovoltaic technologies based on amorphous silicon. Moreover, in this Thesis, with the development of the mentioned goal, differ¬ent techniques of analysis of laser processes have been fine-tuned, basing the same in advanced methods for material characterization (like the combined use of EDX Analysis and Confocal Laser Scanning Microscopy) that can be presented as true breakthroughs in the development of specific techniques for characterization in the study of laser processes of selective ablation of materials in thin film technologies, processes that not only have impact in the photovoltaic field, but also in those of microelectronics, biotechnology, micro-fabrication, etc. As an additional outcome, part of the results of this work has been suc¬cessfully applied, by the investigation group to which the author belongs, to the development of processes of enormous interest within other photo¬voltaic technologies, such as the standard technologies on amorphous silicon over glass in superstrate configuration or the processing of thin layers in conventional technologies using crystalline silicon. Lastly, it is important to mention that this work has been possible thanks to the close cooperation between the Centro L´aser of the UPM, in which the author develops her work, and the Grupo de Silicio Depositado of Centro de Investigaciones Energ´eticas, Medioambientales y Tecnol´ogicas, CIEMAT, which, along with the Grupo de Energ´ıa Fotovoltaica of Univer¬sidad de Barcelona, has prepared the largest part of the samples utilized in this study. Such collaborations have been carried out in the context of several projects of applied investigation with public funding, like Proyecto Singular Estrat´egico PSE-MICROSIL08 (PSE-120000-2006-6), Proyecto IN-NDISOL (IPT-420000-2010-6), both funded by the European Regional De¬velopment Fund (ERDF), ”Una manera de hacer Europa” and MICINN, and the projects of Plan Nacional AMIC (ENE2010-21384-C04-02) and ´ CLASICO (ENE2007-6772-C04-04), whose funds have enabled the devel-opment of large part of this work.