4 resultados para Kaolinite flocculation, Smectite gel, Clay micro-structure

em Universidad Politécnica de Madrid


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The use of fly ash (FA) as an admixture to concrete is broadly extended for two main reasons: the reduction of costs that supposes the substitution of cement and the micro structural changes motivated by the mineral admixture. Regarding this second point, there is a consensus that considers that the ash generates a more compact concrete and a reduction in the size of the pore. However, the measure in which this contributes to the pozzolanic activity or as filler is not well defined. There is also no justification to the influence of the physical parameters, fineness of the grain and free water, in its behavior. This work studies the use of FA as a partial substitute of the cement in concretes of different workability (dry and wet) and the influence in the reactivity of the ash. The concrete of dry consistency which serves as reference uses a cement dose of 250 Kg/m 3 and the concrete of fluid consistency utilized a dose of cement of 350 Kg/m 3 . Two trademark of Portland Cement Type 1 were used. The first reached the resistant class for its fineness of grain and the second one for its composition. Moreover, three doses of FA have been used, and the water/binder ratio was constant in all the mixtures. We have studied the mechanical properties and the micro-structure of the concretes by means of compressive strength tests, mercury intrusion porosimetry (MIP) and thermal analysis (TA). The results of compressive strength tests allow us to observe that concrete mixtures with cements of the same classification and similar dosage of binder do not present the same mechanical behavior. These results show that the effective water/binder ratio has a major role in the development of the mechanical properties of concrete. The study of different dosages using TA, thermo-gravimetry and differential thermal analysis, revealed that the portlandite content is not restrictive in any of the dosages studied. Again, this proves that the rheology of the material influences the reaction rate and content of hydrated cement products. We conclude that the available free water is determinant in the efficiency of pozzolanic reaction. It is so that in accordance to the availability of free water, the ashes can react as an active admixture or simply change the porous distribution. The MIP shows concretes that do not exhibit significant changes in their mechanical behavior, but have suffered significant variation in their porous structure

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This study states the potential trace elements (TE’s) content of red soils located at the centre region of Spain, characterized by low rainfall and slight acidity over prolonged weathering periods. For this purpose, three soil profiles from a catena were described, sampled and analyzed. The most notable characteristics are the low organic matter content and the predominantly acidic pH. Illite and kaolinite are the predominant clay minerals. The fertility of the soils is sufficient to provide most of the nutrients required, with very suitable potassium levels. The geochemical characters of this soil are: only few elements remain almost invariable across the profiles and over time, however the majority of them were directly linked with the clay content. These soils are characterized by relatively low levels of some trace elements such as Sr (64.35 mg?kg–1), Ba (303.67 mg?kg–1) and Sc (13.14 mg?kg–1); high levels of other trace elements such as V (103.92 mg?kg–1), Cr (79.9 mg?kg–1), Cu (15.18 mg?kg–1), Hf (10.26 mg?kg–1), Ni (38 mg?kg–1) and Zr (337 mg?kg–1); while the levels for rare earth elements (REE’s) such as La (48.36 mg?kg–1), Ce (95.07 mg?kg–1), Th (13.33 mg?kg–1) and Nd (42.65 mg?kg–1) are significantly high. The distribution of mayor and trace elements was directly re- lated to weathering processes, parent material and anthropogenic activities.

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The influence of nanosecond laser pulses applied by laser shock peening without absorbent coating (LSPwC) with a Q-switched Nd:YAG laser operating at a wavelength of λ = 1064 nm on 6082-T651 Al alloy has been investigated. The first portion of the present study assesses laser shock peening effect at two pulse densities on three-dimensional (3D) surface topography characteristics. In the second part of the study, the peening effect on surface texture orientation and micro-structure modification, i.e. the effect of surface craters due to plasma and shock waves, were investigated in both longitudinal (L) and transverse (T) directions of the laser-beam movement. In the final portion of the study, the changes of mechanical properties were evaluated with a residual stress profile and Vickers micro-hardness through depth variation in the near surface layer, whereas factorial design with a response surface methodology (RSM) was applied. The surface topographic and micro-structural effect of laser shock peening were characterised with optical microscopy, InfiniteFocus® microscopy and scanning electron microscopy (SEM). Residual stress evaluation based on a hole-drilling integral method confirmed higher compression at the near surface layer (33 μm) in the transverse direction (σmin) of laser-beam movement, i.e. − 407 ± 81 MPa and − 346 ± 124 MPa, after 900 and 2500 pulses/cm2, respectively. Moreover, RSM analysis of micro-hardness through depth distribution confirmed an increase at both pulse densities, whereas LSPwC-generated shock waves showed the impact effect of up to 800 μm below the surface. Furthermore, ANOVA results confirmed the insignificant influence of LSPwC treatment direction on micro-hardness distribution indicating essentially homogeneous conditions, in both L and T directions.

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Los alimentos son sistemas complejos, formados por diversas estructuras a diferentes escalas: macroscópica y microscópica. Muchas propiedades de los alimentos, que son importantes para su procesamiento, calidad y tratamiento postcosecha, están relacionados con su microestructura. La presente tesis doctoral propone una metodología completa para la determinación de la estructura de alimentos desde un punto de vista multi-escala, basándose en métodos de Resonancia Magnética Nuclear (NMR). Las técnicas de NMR son no invasivas y no destructivas y permiten el estudio tanto de macro- como de microestructura. Se han utilizado distintos procedimientos de NMR dependiendo del nivel que se desea estudiar. Para el nivel macroestructural, la Imagen de Resonancia Magnética (MRI) ha resultado ser muy útil para la caracterización de alimentos. Para el estudio microestructural, la MRI requiere altos tiempos de adquisición, lo que hace muy difícil la transferencia de esta técnica a aplicaciones en industria. Por tanto, la optimización de procedimientos de NMR basados en secuencias relaxometría 2D T1/T2 ha resultado ser una estrategia primordial en esta tesis. Estos protocolos de NMR se han implementado satisfactoriamente por primera vez en alto campo magnético. Se ha caracterizado la microestructura de productos alimentarios enteros por primera vez utilizando este tipo de protocolos. Como muestras, se han utilizado dos tipos de productos: modelos de alimentos y alimentos reales (manzanas). Además, como primer paso para su posterior implementación en la industria agroalimentaria, se ha mejorado una línea transportadora, especialmente diseñada para trabajar bajo condiciones de NMR en trabajos anteriores del grupo LPF-TAGRALIA. Se han estudiado y seleccionado las secuencias más rápidas y óptimas para la detección de dos tipos de desórdenes internos en manzanas: vitrescencia y roturas internas. La corrección de las imágenes en movimiento se realiza en tiempo real. Asimismo, se han utilizado protocolos de visión artificial para la clasificación automática de manzanas potencialmente afectadas por vitrescencia. El presente documento está dividido en diferentes capítulos: el Capítulo 2 explica los antecedentes de la presente tesis y el marco del proyecto en el que se ha desarrollado. El Capítulo 3 recoge el estado del arte. El Capítulo 4 establece los objetivos de esta tesis doctoral. Los resultados se dividen en cinco sub-secciones (dentro del Capítulo 5) que corresponden con los trabajos publicados bien en revistas revisadas por pares, bien en congresos internacionales o bien como capítulos de libros revisados por pares. La Sección 5.1. es un estudio del desarrollo de la vitrescencia en manzanas mediante MRI y lo relaciona con la posición de la fruta dentro de la copa del árbol. La Sección 5.2 presenta un trabajo sobre macro- y microestructura en modelos de alimentos. La Sección 5.3 es un artículo en revisión en una revista revisada por pares, en el que se hace un estudio microestrcutural no destructivo mediante relaxometría 2D T1/T2. la Sección 5.4, hace una comparación entre manzanas afectadas por vitrescencia mediante dos técnicas: tomografía de rayos X e MRI, en manzana. Por último, en la Sección 5.5 se muestra un trabajo en el que se hace un estudio de secuencias de MRI en línea para la evaluación de calidad interna en manzanas. Los siguientes capítulos ofrecen una discusión y conclusiones (Capítulo 6 y 7 respectivamente) de todos los capítulos de esta tesis doctoral. Finalmente, se han añadido tres apéndices: el primero con una introducción de los principios básicos de resonancia magnética nuclear (NMR) y en los otros dos, se presentan sendos estudios sobre el efecto de las fibras en la rehidratación de cereales de desayuno extrusionados, mediante diversas técnicas. Ambos trabajos se presentaron en un congreso internacional. Los resultados más relevantes de la presente tesis doctoral, se pueden dividir en tres grandes bloques: resultados sobre macroestructura, resultados sobre microestructura y resultados sobre MRI en línea. Resultados sobre macroestructura: - La imagen de resonancia magnética (MRI) se aplicó satisfactoriamente para la caracterización de macroestructura. En particular, la reconstrucción 3D de imágenes de resonancia magnética permitió identificar y caracterizar dos tipos distintos de vitrescencia en manzanas: central y radial, que se caracterizan por el porcentaje de daño y la conectividad (número de Euler). - La MRI proveía un mejor contraste para manzanas afectadas por vitrescencia que las imágenes de tomografía de rayos X (X-Ray CT), como se pudo verificar en muestras idénticas de manzana. Además, el tiempo de adquisición de la tomografía de rayos X fue alrededor de 12 veces mayor (25 minutos) que la adquisición de las imágenes de resonancia magnética (2 minutos 2 segundos). Resultados sobre microestructura: - Para el estudio de microestructura (nivel subcelular) se utilizaron con éxito secuencias de relaxometría 2D T1/T2. Estas secuencias se usaron por primera vez en alto campo y sobre piezas de alimento completo, convirtiéndose en una forma no destructiva de llevar a cabo estudios de microestructura. - El uso de MRI junto con relaxometría 2D T1/T2 permite realizar estudios multiescala en alimentos de forma no destructiva. Resultados sobre MRI en línea: - El uso de imagen de resonancia magnética en línea fue factible para la identificación de dos tipos de desórdenes internos en manzanas: vitrescencia y podredumbre interna. Las secuencias de imagen tipo FLASH resultaron adecuadas para la identificación en línea de vitrescencia en manzanas. Se realizó sin selección de corte, debido a que la vitrescencia puede desarrollarse en cualquier punto del volumen de la manzana. Se consiguió reducir el tiempo de adquisición, de modo que se llegaron a adquirir 1.3 frutos por segundos (758 ms por fruto). Las secuencias de imagen tipo UFLARE fueron adecuadas para la detección en línea de la podredumbre interna en manzanas. En este caso, se utilizó selección de corte, ya que se trata de un desorden que se suele localizar en la parte central del volumen de la manzana. Se consiguió reducir el tiempo de adquisicón hasta 0.67 frutos por segundo (1475 ms por fruto). En ambos casos (FLASH y UFLARE) fueron necesarios algoritmos para la corrección del movimiento de las imágenes en tiempo real. ABSTRACT Food is a complex system formed by several structures at different scales: macroscopic and microscopic. Many properties of foods that are relevant to process engineering or quality and postharvest treatments are related to their microstructure. This Ph.D Thesis proposes a complete methodology for food structure determination, in a multiscale way, based on the Nuclear Magnetic Resonance (NMR) phenomenon since NMR techniques are non-invasive and non-destructive, and allow both, macro- and micro-structure study. Different NMR procedures are used depending on the structure level under study. For the macrostructure level, Magnetic Resonance Imaging (MRI) revealed its usefulness for food characterization. For microstructure insight, MRI required high acquisition times, which is a hindrance for transference to industry applications. Therefore, optimization of NMR procedures based on T1/T2 relaxometry sequences was a key strategy in this Thesis. These NMR relaxometry protocols, are successfully implemented in high magnetic field. Microstructure of entire food products have been characterized for the first time using these protocols. Two different types of food products have been studied: food models and actual food (apples). Furthermore, as a first step for the food industry implementation, a grading line system, specially designed for working under NMR conditions in previous works of the LPF-TAGRALIA group, is improved. The study and selection of the most suitable rapid sequence to detect two different types of disorders in apples (watercore and internal breakdown) is performed and the real time image motion correction is applied. In addition, artificial vision protocols for the automatic classification of apples potentially affected by watercore are applied. This document is divided into seven different chapters: Chapter 2 explains the thesis background and the framework of the project in which it has been worked. Chapter 3 comprises the state of the art. Chapter 4 establishes de objectives of this Ph.D thesis. The results are divided into five different sections (in Chapter 5) that correspond to published peered reviewed works. Section 5.1 assesses the watercore development in apples with MRI and studies the effect of fruit location in the canopy. Section 5.2 is an MRI and 2D relaxometry study for macro- and microstructure assessment in food models. Section 5.3 is a non-destructive microstructural study using 2D T1/T2 relaxometry on watercore affected apples. Section 5.4 makes a comparison of X-ray CT and MRI on watercore disorder of different apple cultivars. Section 5.5, that is a study of online MRI sequences for the evaluation of apple internal quality. The subsequent chapters offer a general discussion and conclusions (Chapter 6 and Chapter 7 respectively) of all the works performed in the frame of this Ph.D thesis (two peer reviewed journals, one book chapter and one international congress).Finally, three appendices are included in which an introduction to NMR principles is offered and two published proceedings regarding the effect of fiber on the rehydration of extruded breakfast cereal are displayed. The most relevant results can be summarized into three sections: results on macrostructure, results on microstructure and results on on-line MRI. Results on macrostructure: - MRI was successfully used for macrostructure characterization. Indeed, 3D reconstruction of MRI in apples allows to identify two different types of watercore (radial and block), which are characterized by the percentage of damage and the connectivity (Euler number). - MRI provides better contrast for watercore than X-Ray CT as verified on identical samples. Furthermore, X-Ray CT images acquisition time was around 12 times higher (25 minutes) than MRI acquisition time (2 minutes 2 seconds). Results on microstructure: - 2D T1/T2 relaxometry were successfully applied for microstructure (subcellular level) characterization. 2D T1/T2 relaxometry sequences have been applied for the first time on high field for entire food pieces, being a non-destructive way to achieve microstructure study. - The use of MRI together with 2D T1/T2 relaxometry sequences allows a non-destructive multiscale study of food. Results on on-line MRI: - The use of on-line MRI was successful for the identification of two different internal disorders in apples: watercore and internal breakdown. FLASH imaging was a suitable technique for the on-line detection of watercore disorder in apples, with no slice selection, since watercore is a physiological disorder that may be developed anywhere in the apple volume. 1.3 fruits were imaged per second (768 ms per fruit). UFLARE imaging is a suitable sequence for the on-line detection of internal breakdown disorder in apples. Slice selection was used, as internal breakdown is usually located in the central slice of the apple volume. 0.67 fruits were imaged per second (1475 ms per fruit). In both cases (FLASH and UFLARE) motion correction was performed in real time, during the acquisition of the images.