Desarrollo de nuevas metodologías analíticas para el control de procesos y productos industriales : aplicación de la espectroscopia NIR y la espectrometría de movilidad iónica (IMS) /

La industria en general, y particularmente la química y la farmacéutica, necesita mejorar la eficiencia de los procesos de producción, para asegurar la obtención de productos con una elevada calidad y a la vez reducir consumos, lo que redundará en una mejora de la productividad. Esta demanda precisa del desarrollo de metodologías analíticas simples, rápidas, fiables y de bajo coste, que puedan ser utilizadas en rutina y por personal poco cualificado, que posibiliten realizar un seguimiento de todo el proceso de producción, y si es necesario aplicar las medidas correctivas necesarias, con el objeto de obtener productos de elevada calidad. Con el objetivo de proporcionar a la industria nuevas metodologías de análisis que permitan cumplir con estos objetivos, en esta tesis se han realizado diversos estudios basados en la espectroscopia NIR y la espectrometría de movilidad iónica (IMS). En el primer estudio de la tesis se ha aplicado la espectroscopia NIR para la monitorización in-line de un proceso de esterificación enzimática de glicerina con ácido esteárico en presencia de una lipasa de Candida Antarctica, mediante la inmersión de una sonda NIR en el reactor. En los diferentes procesos realizados, la reacción enzimática conduce a la formación de diestearato y monoestearato de glicerina; no se observa la formación de triestearato. Se han desarrollado modelos de calibración PLS para cada uno de los componentes, usando los espectros registrado y los valores obtenidos por cromatografía de permeación en gel; los modelos son simples y presentan una correcta capacidad predictiva. Los métodos desarrollados se han aplicado al seguimiento de otros procesos obteniendo resultados que demuestran la utilidad del NIR en la monitorización in-line de la reacción de esterificación enzimática estudiada. El siguiente estudio ha consistido en el desarrollo de un método NIR para la determinación de los componentes de una mezcla adyuvante para un herbicida que se aplica por pulverización de una suspensión. La gran semejanza de los espectros de algunos componentes ha exigido la aplicación de un diseño experimental para la preparación de muestras, que tiene por objeto asegurar la robustez del modelo de calibración. La aplicación de los modelos construidos a muestras de lotes de producción, mostró la buena capacidad predictiva de los modelos construidos y su utilidad para controlar la composición de este tipo de mezclas. En un tercer trabajo se desarrollaron bibliotecas espectrales para la identificación de formulaciones lubricantes, que presentan espectros muy similares. El método desarrollado basado en la construcción de bibliotecas en cascada o sub-bibliotecas permite asegurar la especificidad necesaria para la discriminación entre productos que la biblioteca general identifica ambiguamente. Utilizando criterios de diferenciación más estrictos la biblioteca permite la diferenciación de formulaciones lubricantes que contienen o no aditivos en un porcentaje relativamente pequeño (0.05-0.7%). En este trabajo también se construyeron modelos PLS para la determinación de composición y viscosidad de los lubricantes. En esta tesis se han desarrollado métodos analíticos utilizando la técnica IMS, por primera vez en nuestro grupo de investigación, con el objeto de complementar algunos aspectos analíticos que no se pueden resolver mediante NIR y que son asequibles a la espectrometría de Movilidad Iónica (IMS). Esta es una nueva técnica nueva que ha sido escasamente utilizada en la industria química y farmacéutica. Se han estudiado, desarrollado y validado dos nuevos métodos analíticos, para la determinación de amina residual a lo largo del proceso de fabricación de amidoaminas y fosfolípidos, y otro para la determinación de dos principios activos (en una baja concentración) de un preparado farmacéutico. En ambos casos se han estudiado la influencia de los factores instrumentales en la respuesta IMS y realizando una optimización del método de cuantificación para conseguir la mejor respuesta instrumental y sensibilidad. Se han construido modelos multivariables que permiten la determinación de las especies de interés. Los métodos desarrollados se han aplicado al control analítico de los preparados estudiados.The industry, and particularly chemistry and pharmaceuticals, needs to improve the efficiency of production processes to ensure obtaining the products in high quality while reducing consumption, what will result in improving productivity. This demand requires the development of analytical methodologies in simple, fast, reliable and low cost manner, which can be used in routine and by unskilled labor, which enable to track the entire production process, and if necessary, apply corrective actions, to obtain high quality products. In order to provide the industry these new methods of analysis to achieve these objectives, in this thesis there have been carried out several studies based on NIR spectroscopy and ion mobility spectrometry (IMS). In the first study of the thesis, NIR spectroscopy has been applied for in-line monitoring of enzymatic esterification process of glycerol with stearic acid in the presence of a lipase from Candida Antarctica, with a NIR immersion probe in the reactor. In the processes performed, the enzymatic reaction leads to the formation of glycol distearate and glycerol monostearate; not being observed the formation of tristearate. It has been developed PLS calibration models for each of the components, using the spectra recorded and the values obtained by gel permeation chromatography; the models were simple and had a correct prediction. The developed methods have been applied to monitoring processes, obtaining results that demonstrate the usefulness of NIR in-line monitoring of the enzymatic esterification reaction studied. The next study involved the development of a NIR method for determining components of a mixture adjuvant in an herbicide product, which was applied for spraying a suspension. The great similarity of the components spectra has required the implementation of an experimental design for sample preparation, which aim is to ensure robustness of the calibration model. The application of the models built to samples of production batches showed good predictive ability of the models constructed, and their utility for checking the composition of such mixtures. In a third work, spectral libraries were developed for the identification of lubricant formulations, which had very similar spectra. The developed method based on the construction of libraries or sub-cascading libraries, ensures the necessary specificity for discrimination between products that were unambiguously identified in the general library. Using more stringent criteria of differentiation, the library allows the differentiation between lubricant formulations which contain or not additives in a relatively small amount (0.05 to 0.7%). In this work, PLS models were also constructed for the determination of composition and viscosity of lubricants. In the present thesis, we have developed analytical methods using IMS technique for the first time in our research group, in order to complement some analytical issues that cannot be resolved by NIR and that are amenable to IMS. This is a new technique that has been rarely used in the chemical and pharmaceutical industries. There have been studied, developed and validated two new analytical methods for determination of residual amine during the manufacturing process of amidoamines and phospholipids, and one for the determination of two active principles ingredients (in low concentration) of a pharmaceutical preparation. In both cases, we have studied the influence of instrumental factors in the IMS response and we have performed an optimization of the quantification method to get the best instrumental response and sensitivity. Multivariate models were constructed which allowed the determination of the species of interest. The developed methods have been applied to analytical control of the preparations studied

I Congreso Nacional de Cofradías de Semana Santa : [actas]

BibliografíaCopia digital. Valladolid : Junta de Castilla y León. Consejería de Cultura y Turismo, 2009-201

Chemical characterization of an encapsulated red wine powder and its effects on neuronal cells

Red wine polyphenols are known for their implications for human health protection, although they suffer from high instability. For this reason, a red wine powder was prepared by freeze-drying encapsulation in maltodextrin/arabic gum matrix, and its composition was determined by means of high-performance liquid chromatography coupled quadrupole time-of-flight mass spectrometry (HPLC-MS-QTOF). More than thirty polyphenols, including anthocyanins, flavanols, flavonols, phenolic acids and stilbenoids, were identified. Some of the main quantified polyphenols were: malvidin-3-O-glucoside, malvidin 3-O-(6”-acetyl-glucose), petunidin-3-O-glucoside, quercetin-3-O-glucuronide, syringenin-3-O-glucoside, epicatechin, gallic acid and syringic acid. The biological activity of this de-alcoholized and encapsulated red wine on human neuroblastoma SH-SY5Y cells was studied. The results showed that the encapsulated red wine powder has active redox properties, as verified by performing reactive oxygen species (ROS) analysis utilizing a neuronal model. This could help explain its action against the neurotoxicity induced by 6-hydroxydopamine (6-OHDA).Fil: Rocha Parra, Diego Fernando. Consejo Superior de Investigaciones Científicas. Instituto de Ciencia y Tecnologia de Alimentos y Nutrición; España. Pontificia Universidad Católica Argentina "Santa María de los Buenos Aires"; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; ArgentinaFil: Chirife, Jorge. Pontificia Universidad Católica Argentina "Santa María de los Buenos Aires"; ArgentinaFil: Zamora, María Clara. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Pontificia Universidad Católica Argentina "Santa María de los Buenos Aires"; ArgentinaFil: de Pascual Teresa, Sonia. Consejo Superior de Investigaciones Científicas. Instituto de Ciencia y Tecnologia de Alimentos y Nutrición; Españ

Operating Point Optimization of a Hydrogen Fueled Hybrid Solid Oxide Fuel Cell-Steam Turbine (SOFC-ST) Plant

This paper presents a hydrogen powered hybrid solid oxide fuel cell-steam turbine (SOFC-ST) system and studies its optimal operating conditions. This type of installation can be very appropriate to complement the intermittent generation of renewable energies, such as wind generation. A dynamic model of an alternative hybrid SOFC-ST configuration that is especially suited to work with hydrogen is developed. The proposed system recuperates the waste heat of the high temperature fuel cell, to feed a bottoming cycle (BC) based on a steam turbine (ST). In order to optimize the behavior and performance of the system, a two-level control structure is proposed. Two controllers have been implemented for the stack temperature and fuel utilization factor. An upper supervisor generates optimal set-points in order to reach a maximal hydrogen efficiency. The simulation results obtained show that the proposed system allows one to reach high efficiencies at rated power levels.This work has been carried out in the Intelligent Systems and Energy research group of the University of the Basque Country (UPV/EHU) and has been supported by the UFI11/28 research grant of the UPV/EHU and by the IT677-13 research grant of the Basque Government (Spain) and by DPI2012-37363-CO2-01 research grant of the Spanish Ministry of Economy and Competitiveness

Destination image, satisfaction and destination and loyalty in cruise tourism: the case of Málaga (Spain)

Over the past decades cruise tourism is a sector that has experienced a tremendous growth around the globe. The relations that are established between the different agents that interact in this industry, passengers, crew and residents are crucial for visitor satisfaction and the success of the tourist destination. The study has analyzed the different types of cruise passengers who landed at the port of Malaga and their perception of the city through destination image, satisfaction and destination loyalty. A cluster analysis identified the existence of four different groups of passengers whose opinions can give a specific answer to the consolidation of Malaga as a quality tourist destination. From a practical point of view, recommendations about the adequate management of the destination´s attractions for the cruise industry are discussed in the conclusions.Universidad de Málaga. Campus de Excelencia Internacional Andalucía Tec

Reglamento para la administración y régimen interior del mercado

Copia digital. Valladolid : Junta de Castilla y León. Consejería de Cultura y Turismo, 2009-201

ADAPTS: An Intelligent Sustainable Conceptual Framework for Engineering Projects

This paper presents a conceptual framework for the optimization of environmental sustainability in engineering projects, both for products and industrial facilities or processes. The main objective of this work is to propose a conceptual framework to help researchers to approach optimization under the criteria of sustainability of engineering projects, making use of current Machine Learning techniques. For the development of this conceptual framework, a bibliographic search has been carried out on the Web of Science. From the selected documents and through a hermeneutic procedure the texts have been analyzed and the conceptual framework has been carried out. A graphic representation pyramid shape is shown to clearly define the variables of the proposed conceptual framework and their relationships. The conceptual framework consists of 5 dimensions; its acronym is ADAPTS. In the base are: (1) the Application to which it is intended, (2) the available DAta, (3) the APproach under which it is operated, and (4) the machine learning Tool used. At the top of the pyramid, (5) the necessary Sensing. A study case is proposed to show its applicability. This work is part of a broader line of research, in terms of optimization under sustainability criteria.Telefónica Chair “Intelligence in Networks” of the University of Seville (Spain

A fast ethanol assay to detect seed deterioration

The most common way to test seed quality is to use a simple and reliable but time- and space-consuming germination test. In this paper we present a fast and simple method to analyse cabbage seed deterioration by measuring ethanol production from partially imbibed seeds. The method uses a modified breath analyser and is simple compared to gas chromatographic or enzymatic procedures. A modified method using elevated temperatures (40°C instead of 20°C) shortened the assay time and improved its sensitivity. The analysis showed an inverse correlation between ethanol production and seed quality (e.g. the final percentages or speed of germination and the number of normal seedlings). The increase in ethanol production was observed when cabbage seeds were deteriorated by storage under ambient conditions or hot water treatments, both of which reduced the number of normal seedlings. Premature seeds produced more ethanol upon imbibition than mature seeds. Ethanol production occurred simultaneously with oxygen consumption, indicating that lack of oxygen is not the major trigger for ethanol production

Sellos de pan : [exposición, Casa de Cultura de Zamora, del 25 de junio al 27 de julio de 1986]

Copia digital. Valladolid : Junta de Castilla y León. Consejería de Cultura y Turismo, 2009-201