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Sepiolite is a clay mineral, a complex magnesium silicate, a typical formula for which is (OH2)4(OH)4Mg8Si12O30•8H2O. It is formed by blocks and cavities (tunnels) growing in the direction of the fibres. The tunnels, 3.7 x 10.6 Å in cross-section, are responsible for the high specific surface area and sorptive properties of sepiolite. The co-intercalation of 3-methyl cyclohex-2-en-1-one (MCH), the Douglas-Fir beetle anti-aggregation pheromone, with methanol, ethanol, acetone, or benzene into sepiolite tunnels was studied. The resulting nanohybrid materials were characterized by means of various techniques, such as multinuclear solid-state NMR spectroscopy, porosity studies and Thermal Gravimetric Analysis (TGA). This was done in the hope of obtaining slow and controlled release of MCH from the sepiolite tunnels. It was demonstrated by 13C MAS NMR (carbon-13 magic angle spinning nuclear magnetic resonance) that at room temperature there are two different MCH molecules: one MCH inside the tunnels and the other one outside the tunnels of the sepiolite. Heating nanohybrid materials at 60˚C for 20 hours removes the external MCH molecules from the sepiolite. 13C MAS NMR showed that by further heating nanohybrid materials at 120˚C for 20 hours, methanol, ethanol, or acetone peaks were greatly reduced; however, the benzene peak was not reduced. To better understand how benzene acts inside sepiolite, intercalation of d6-benzene, and co-intercalations of d6-benzene with MCH and d6-benzene with pyridine into sepiolite tunnels were carried out, and these samples were studied by the same techniques. Another technique was used in order to see whether the slow and controlled release of MCH from the sepiolite tunnels could be obtained: sepiolite-MCH nanohybrids were treated with 20 ml of 0.5 M HCl solution. It was found that when 1 gram of MCH-sepiolite sample was acid treated at room temperature, about 35% of intercalated MCH was removed from the sepiolite. The role of sepiolite clay was also studied in Maya-Blue representative structure sepiolite-indigo adduct. It is known that upon heating the sepiolite and indigo mixture, the stability that is present in Maya-Blue is achieved. It is still a mystery, however, how exactly indigo and sepiolite interact with each other.

Sepiolite is a clay mineral, a complex magnesium silicate, a typical formula for which is (OH2)4(OH)4Mg8Si12O30•8H2O. It is formed by blocks and cavities (tunnels) growing in the direction of the fibres. The tunnels, 3.7 x 10.6 Å in cross-section, are responsible for the high specific surface area and sorptive properties of sepiolite. The co-intercalation of 3-methyl cyclohex-2-en-1-one (MCH), the Douglas-Fir beetle anti-aggregation pheromone, with methanol, ethanol, acetone, or benzene into sepiolite tunnels was studied. The resulting nanohybrid materials were characterized by means of various techniques, such as multinuclear solid-state NMR spectroscopy, porosity studies and Thermal Gravimetric Analysis (TGA). This was done in the hope of obtaining slow and controlled release of MCH from the sepiolite tunnels. It was demonstrated by 13C MAS NMR (carbon-13 magic angle spinning nuclear magnetic resonance) that at room temperature there are two different MCH molecules: one MCH inside the tunnels and the other one outside the tunnels of the sepiolite. Heating nanohybrid materials at 60˚C for 20 hours removes the external MCH molecules from the sepiolite. 13C MAS NMR showed that by further heating nanohybrid materials at 120˚C for 20 hours, methanol, ethanol, or acetone peaks were greatly reduced; however, the benzene peak was not reduced. To better understand how benzene acts inside sepiolite, intercalation of d6-benzene, and co-intercalations of d6-benzene with MCH and d6-benzene with pyridine into sepiolite tunnels were carried out, and these samples were studied by the same techniques. Another technique was used in order to see whether the slow and controlled release of MCH from the sepiolite tunnels could be obtained: sepiolite-MCH nanohybrids were treated with 20 ml of 0.5 M HCl solution. It was found that when 1 gram of MCH-sepiolite sample was acid treated at room temperature, about 35% of intercalated MCH was removed from the sepiolite. The role of sepiolite clay was also studied in Maya-Blue representative structure sepiolite-indigo adduct. It is known that upon heating the sepiolite and indigo mixture, the stability that is present in Maya-Blue is achieved. It is still a mystery, however, how exactly indigo and sepiolite interact with each other.

Sepiolite is a clay mineral, a complex magnesium silicate, a typical formula for which is (OH2)4(OH)4Mg8Si12O30•8H2O. It is formed by blocks and cavities (tunnels) growing in the direction of the fibres. The tunnels, 3.7 x 10.6 Å in cross-section, are responsible for the high specific surface area and sorptive properties of sepiolite. The co-intercalation of 3-methyl cyclohex-2-en-1-one (MCH), the Douglas-Fir beetle anti-aggregation pheromone, with methanol, ethanol, acetone, or benzene into sepiolite tunnels was studied. The resulting nanohybrid materials were characterized by means of various techniques, such as multinuclear solid-state NMR spectroscopy, porosity studies and Thermal Gravimetric Analysis (TGA). This was done in the hope of obtaining slow and controlled release of MCH from the sepiolite tunnels. It was demonstrated by 13C MAS NMR (carbon-13 magic angle spinning nuclear magnetic resonance) that at room temperature there are two different MCH molecules: one MCH inside the tunnels and the other one outside the tunnels of the sepiolite. Heating nanohybrid materials at 60˚C for 20 hours removes the external MCH molecules from the sepiolite. 13C MAS NMR showed that by further heating nanohybrid materials at 120˚C for 20 hours, methanol, ethanol, or acetone peaks were greatly reduced; however, the benzene peak was not reduced. To better understand how benzene acts inside sepiolite, intercalation of d6-benzene, and co-intercalations of d6-benzene with MCH and d6-benzene with pyridine into sepiolite tunnels were carried out, and these samples were studied by the same techniques. Another technique was used in order to see whether the slow and controlled release of MCH from the sepiolite tunnels could be obtained: sepiolite-MCH nanohybrids were treated with 20 ml of 0.5 M HCl solution. It was found that when 1 gram of MCH-sepiolite sample was acid treated at room temperature, about 35% of intercalated MCH was removed from the sepiolite. The role of sepiolite clay was also studied in Maya-Blue representative structure sepiolite-indigo adduct. It is known that upon heating the sepiolite and indigo mixture, the stability that is present in Maya-Blue is achieved. It is still a mystery, however, how exactly indigo and sepiolite interact with each other.

Sepiolite is a clay mineral, a complex magnesium silicate, a typical formula for which is (OH2)4(OH)4Mg8Si12O30•8H2O. It is formed by blocks and cavities (tunnels) growing in the direction of the fibres. The tunnels, 3.7 x 10.6 Å in cross-section, are responsible for the high specific surface area and sorptive properties of sepiolite. The co-intercalation of 3-methyl cyclohex-2-en-1-one (MCH), the Douglas-Fir beetle anti-aggregation pheromone, with methanol, ethanol, acetone, or benzene into sepiolite tunnels was studied. The resulting nanohybrid materials were characterized by means of various techniques, such as multinuclear solid-state NMR spectroscopy, porosity studies and Thermal Gravimetric Analysis (TGA). This was done in the hope of obtaining slow and controlled release of MCH from the sepiolite tunnels. It was demonstrated by 13C MAS NMR (carbon-13 magic angle spinning nuclear magnetic resonance) that at room temperature there are two different MCH molecules: one MCH inside the tunnels and the other one outside the tunnels of the sepiolite. Heating nanohybrid materials at 60˚C for 20 hours removes the external MCH molecules from the sepiolite. 13C MAS NMR showed that by further heating nanohybrid materials at 120˚C for 20 hours, methanol, ethanol, or acetone peaks were greatly reduced; however, the benzene peak was not reduced. To better understand how benzene acts inside sepiolite, intercalation of d6-benzene, and co-intercalations of d6-benzene with MCH and d6-benzene with pyridine into sepiolite tunnels were carried out, and these samples were studied by the same techniques. Another technique was used in order to see whether the slow and controlled release of MCH from the sepiolite tunnels could be obtained: sepiolite-MCH nanohybrids were treated with 20 ml of 0.5 M HCl solution. It was found that when 1 gram of MCH-sepiolite sample was acid treated at room temperature, about 35% of intercalated MCH was removed from the sepiolite. The role of sepiolite clay was also studied in Maya-Blue representative structure sepiolite-indigo adduct. It is known that upon heating the sepiolite and indigo mixture, the stability that is present in Maya-Blue is achieved. It is still a mystery, however, how exactly indigo and sepiolite interact with each other.

The proportion of authigenic to detrital clay minerals in terrestrial sediments is variable. It has previously been hypothesized that pure Mg-silicates in regions such as Amboseli Basin in Kenya occur due to the absence of Al-rich detritus. We tested this by replicating two Mg-silicate synthesis experiments while adding Al-rich smectite. The first study produced an X-ray amorphous Mg-silicate gel, with little response to addition of Al-rich smectite. The second experiment shifted the 060 peak associated with clay octahedral sheets, suggesting we synthesized trioctahedral domains in a smectite structure. Peak height increased linearly with more heating, indicating crystallinity changes. These results confirm that Al-rich detritus can influence the mineralogy of authigenic clays in saline, alkaline settings. By examining how clay neoformation is affected by silica saturation, we can better understand how the clays found in Neogene lacustrine environments are formed and the climate and of that time.

The voltammetric behavior of selected nitrophenols (2-nitrophenol, 4-nitrophenol, 2,4-dinitrophenol and 2,4,6-trinitrophenol) was investigated by differential pulse voltammetry (DPV) and by adsorptive stripping voltammetry (AdSV) at an unmodified electrode (CPE) and a clay-modified carbon paste electrodes modified by montmorillonite (MMT-CPE) and sepiolite (SEP-CPE) using electrochemical reduction and oxidation in Britton-Robinson buffer. For reduction, optimum conditions have been found at pH 2 for 2-NP and 4-NP, at pH 3 for 2,4-DNP and at pH 4 for 2,4,6-TNP. For oxidation, optimum conditions have been found at pH 2 for 2-NP and 4-NP and at pH 5 for 2,4-DNP. Voltammetric determination using electrochemical oxidation is not a suitable method for 2,4,6-TNP. The lowest detection limits were obtained for 2-NP using cathodic AdSV on SEP-CPE with 2,9·10-7 mol.dm-3 , for 4-NP using cathodic DPV on MMT-CPE with 2·10-6 mol.dm-3 , for 2,4-DNP using cathodic AdSV on SEP-CPE with 2,7·10-7 mol.dm-3 and for 2,4,6-TNP using cathodic DPV on unmodified electrode with 4,8·10-7 mol.dm-3 . Determination of mixture 2-NP and 4-NP and the possibility of the selective determination using open circuit sorption with DPV detection was further studied.

Master of Science / Food Science Institute / Jayendra Amamcharla / Greek yogurt is one of the largest-growing sectors in the dairy industry accounting for over 25% of yogurt sales in the United States. Greek yogurt is produced by removing a portion of water and water soluble components from yogurt. Consequently, a large quantity of Greek yogurt whey (GYW) is being produced as a co-product. GYW is compositionally different from cheese whey, and thus poses economic and environmental challenges to the dairy industry. The objective of the present study was to evaluate two physical treatments as alternative methods for separating valuable GYW components: magnetic fluid treatment (MFT) and the addition of sepiolite, a clay mineral. A MFT chamber was designed using four pairs of neodymium magnets arranged to produce a magnetic field strength of 0.6 Tesla. Three batches of GYW each from two manufacturers were procured. A 2×3 factorial design was used with MFT or without MFT and the addition of zero, two, or four grams of sepiolite per 100g of GYW. The pH of GYW was adjusted to 7.2 using 5N NaOH solution, and the GYW was pumped at a rate of 7.5 L/min through the MFT system with or without MFT chamber attached. The sample was split into three sub-samples, heated to 80°C, and sepiolite was added as per the experimental design. The samples were centrifuged at 1,000g for five minutes. The top aqueous layer was separated and analyzed for total solids, ash, lactose, protein, calcium, phosphates, and sodium content along with color. MFT did not influence the analyzed whey components (P > 0.05) except for lactose. However, addition of sepiolite influenced protein content and a* and b* color values for the top aqueous layers (P < 0.05). Both levels of sepiolite addition resulted in about a 50% decrease in protein compared to original GYW. Adding two grams of Sepiolite per 100g of GYW from manufacturer 1 resulted in b* decreasing from 25.99 to 8.16 compared to treated GYW with no sepiolite. Sepiolite was found to have possible applications in the removal of proteins and color pigments in GYW.

L'électrorhéologie est un domaine où les possibilités d'accroître les performances en utilisant des composés hybrides organiques-inorganiques ont été explorées. Les fluides électrorhéologiques sont des dispersions de particules colloïdales facilement polarisables par un champ électrique dans un liquide non conducteur. Lorsqu'un champ électrique est appliqué les propriétés rhéologiques changent et la viscosité apparente peut augmenter ou diminuer en fonction du type de particules présentes dans le fluide. Ces fluides appartiennent à la classe des matériaux intelligents qui ont un grand potentiel technologique avec des applications dans de nombreux domaines comme l'automobile, l'hydraulique, les joints d'étanchéité, la robotique, le spatial et même en médecine. Dans ce travail on s'intéresse à trois différentes sortes d'hybride: des silicates avec des molécules organiques (ORMOSIL) modifiés par des groupements mercaptan, des liquides ioniques encapsulés dans la silice, et des fibres de sépiolite recouvertes de polyaniline. Pour la synthèse des particules à base de silice (ORMOSIL) et les liquides ioniques encapsulés dans la silice, on a utilisé le procédé sol-gel. Dans le cas de la polyaniline sur la sépiolite, deux méthodes de polymérisation ont été utilisées: en phase solide et en suspension. Tous les systèmes étudiés ont présenté une réponse électrorhéologique. Parmi eux l'hybride polyaniline/sépiolite a fourni la meilleure réponse électrorhéologique, sans doute à cause de la forme allongée des particules, qui donne une contrainte seuil plus grande que les formes sphériques obtenues pour les hybrides à base de silice. / Electrorheology is an area has been exploring the application of these organic-inorganic hybrid compounds, to obtain better performance in electrorheological properties. Electro-rheological fluids consist of a colloidal dispersion, where the liquid is non-conductive and the particles dispersed in the fluid are able of polarized at presence of electric field. When the fluids ER are subjected to an external electric field the rheological properties change, and may increase or decrease the apparent viscosity, it depending on the type of particle present in the fluid. These fluids fall into the class of smart materials witch were of great technological interest, since they are finding applications in: automotive industrial, hydraulics industrial, fluid sealing, robots, aerospace and medicine, among others. In this work were discussed three different kinds of hybrids: organically modified silanes (ORMOSIL) modified with mercaptans groups, ionic liquid encapsulated by silica and sepiolite fibers coated by polyaniline. For the synthesis of particles concerned silica (ORMOSIL and ionic liquid encapsulated by silica) the sol-gel process was used. In the case of polyaniline and sepiolite two synthetic methods of polymerization were applied: bulk and slurry. All systems studied presented electrorheological response. Among them, the polyaniline/sepiolite hybrid materials was provided the best electrorheological response, probably due to its elongated morphology supplied the yield stress greater than spherical morphologies, which were obtained for silica hybrids.

Orientadora: Profa. Dra. Sandra Andrea Cruz / Tese (doutorado) - Universidade Federal do ABC, Programa de Pós-Graduação em Nanociências e Materiais Avançados, 2015. / A principal proposta desse estudo foi o desenvolvimento, compatibilização e caracterização de (nano)compósitos de polipropileno com a argila sepiolita. Na primeira etapa a sepiolita foi analisada e estudada por meio de diferentes técnicas. As análises químicas mostraram que a sua estrutura é composta predominantemente por átomos de silício e os resultados de espectroscopia mostraram a presença de grupos silanois e hidroxilas na sua estrutura. O estudo térmico da argila permitiu um maior entendimento sobre o perfil de perda de massa e das alterações que ocorrem em sua estrutura, quando aquecida. Ainda, os resultados indicaram que a sua área superficial específica apresentou ser elevada, com valores próximos aos já relatados na literatura. Na segunda etapa foram sintetizados dois agentes compatibilizantes a partir do PP virgem, no estado fundido: glicidil metacrilato (GMA) para produzir o PP-GMA e o viniltrietoxisilano (VTES) foi utilizado para sintetizar o PP-VTES. Os resultados das análises químicas mostraram que foi possível funcionalizar o PP com os diferentes grupos pendentes através da metodologia proposta. Através das análises térmicas os resultados mostraram que a síntese do PP com GMA ou VTES na presença de DCP vem acompanhada predominantemente de reações de cisão de cadeia. As análises reológicas mostraram que esses processos degradativos foram responsáveis pela diminuição da massa molar, sendo que para o PP-VTES este efeito foi mais pronunciado. Em uma etapa final estudou-se a influência de diferentes concentrações de PP-GMA ou PP-VTES e/ou SEP no PP. De uma maneira geral, pôde-se concluir através das análises reológicas, químicas, morfológicas e mecânicas que, apesar dos agentes compatibilizantes promoverem uma maior molhabilidade da carga pela matriz, como indicado pelas análises de MEV, as alterações não foram significativas ao ponto de se atribuir os resultados obtidos ao efeito que seria esperado para uma elevada dispersão e interação das agulhas ou fibras de SEP com a matriz de PP. / The main purpose of this study was the development, compatibilization, and characterization of polypropylene and sepiolite clay nanocomposites. In the first stage, the sepiolite was analyzed and studied using different techniques. The chemical analyses showed that it is mainly composed of silicon atoms, while the spectroscopy results indicated the presence of silanol and hydroxyl groups in its structure. The thermal study of the clay enabled better understanding of the mass-loss profile and the changes that took place in its structure when heated. Also, the results indicated that its specific surface area was high, with values close to those reported in the literature. In the second stage, two compatibilizing agents were synthesized from pristine molten PP: glycidyl methacrylate (GMA) to produce PP-GMA; and vinyltrimethoxysilane (VTES) to synthesize PP-VTES. The chemical analysis results showed that it was possible to functionalize the PP with the different pending groups through the proposed methodology. The results from the thermal analyses showed that the synthesis of the PP with GMA or VTES, in the presence of DCP, is predominantly accompanied by chain scission reactions. The rheological analyses showed that these degrading processes were responsible for the molar mass reduction ¿ for the PP-VTES this effect was more pronounced. In the final stage, the influence of different concentrations of PP-GMA or PP-VTES and/or SEP on the PP was studied. From a general point of view, through the rheological, chemical, morphological, and mechanical analyses it can be concluded that, despite the compatibilizing agents promoting greater wettability of the batch via the matrix ¿ as indicated by the MEV analyses ¿ the alterations were not significant to the point of attributing the results obtained to the effect that would be expected for an elevated dispersion and interaction of the SEP needles or fibers with the PP matrix.