Bioethanol is a promising renewable biofuel and wheat is currently the main candidate asthe feedstock for its production in the UK context. The quality of the numerous varieties ofwheat developed in the past by plant breeders has been well examined in terms of bread, biscuitand pasta producing industries. In general, the end-use quality determination of wheat in termsof alcohol yield is less investigated. This work focused on understanding and predicting thealcohol yield from wheat according to its physical, physicochemical and chemicalcharacteristics. The research ran alongside the GREEN Grain project and utilised its wheatsamples, which consist of a range of wheat varieties, agronomic regimes and growing sitesfrom four harvests years 2005-2008. The combined dataset consists of a diverse range ofchemical, physicochemical and physical characteristics of the GREEN Grain wheats. An initial multivariate analysis (PCA) indicated that the first principal component, whichexplains most of the variability of the wheat characteristics, is related with the classification ofwheat as hard or soft. High alcohol yielding wheats typically have high starch, mealiness andalbumin+globulin fraction, and also low protein, gliadin fraction and hardness. They also havelarger and more spherical kernels. Analysis of Variance (ANOVA) was applied in order to identify differences between thevarieties, the sites and the application or not of N fertiliser. The ANOVA showed that theapplication of N fertiliser increases all the protein components, although it increases the Gliadinand the LMW glutenins more. N fertiliser also yields smaller (TGW, width, depth) and moreelongated kernels. High alcohol yielding varieties tend to be softer with lower protein andlarger and more spherical kernels. This consistent variability allowed prediction of the alcoholyield based on easily measured parameters. The following model, based on the SKCS reportedvalues plus protein, could predict the alcohol yield with an R2 of about 78%:Alcohol yield = 466.62 - 5.07 × Protein - 0.21 × hardness + 11.6 × diameter ±6.94 l/dry tonIt is frequently hypothesised that larger and more rounded kernels produce more alcoholbecause they have a smaller relative amount of the unfermentable outer layers. In an effort totest this hypothesis, the pericarp thicknesses and the crease characteristics of the wheat sampleswere measured. It was found that pericarp thickness and crease dimensions vary with kernelsize, with significant differences between varieties. A physical model was developed thatconsiders these differences and calculates the endosperm to non-endosperm ratio. None of thevariables obtained by the physical model could be related to alcohol yield. The SKCS fundamental data were further analysed in an effort to improve the alcoholyield predictability. It was found that the averaged Crush Response Profiles are morereproducible than the hardness index itself. It was shown that the initial peak does not occurbecause of the "shell" (i.e. the bran layers) as suggested in the literature, but because of thecrease. Examination of the effects of moisture content on the aCRPs showed that their 1stquarter is equivalent to the stress-strain plots of dedicated rheological tests. The remaining partsof the curve relate to the post-failure behaviour of the kernels and with hardness as used incereal science. The aCRP parameters could improve the alcohol yield predictability of theGREEN Grain wheats to an R2 of about 82.3% and a standard error of the regression of6.3 l/dry ton. Further standardisation and calibration with respect to the moisture content and tothe size of the kernels could improve the predictions even further. Textural testing of cereals is constrained by the complexity of the wheat kernel structureand exacerbated by the between-kernel variation. The current work has demonstrated howSKCS data can be interpreted more insightfully in order to improve end-use quality predictions. The aCRP parameters clearly contain rheological information about wheats. Further research toestablish their examination by more standardised methodologies will allow effectiveinvestigation of connections between the rheological properties, chemical characteristics,processing behaviour and end-use quality prediction of wheat.

<p>Uprkos brojnim tradicionalnim reolo&scaron;kim metodama koje se već dugi niz godina koriste u proceni kvaliteta bra&scaron;na, postoji potreba za razvijanjem novih metoda, pomoću kojih bi se za kratko vreme i uz ograničenu količinu uzorka mogao uspe&scaron;no predvideti kvalitet bra&scaron;na i gotovog proizvoda. Na taj način selekcionerima bi bila omogućena procena tehnolo&scaron;kog kvaliteta linija p&scaron;enice čija je količina ograničena, dok bi se mlinarima obezbedio brz metod procene kvaliteta. Osnovni cilj istraživanja ove disertacije je ispitivanje mogućnosti primene novog reolo&scaron;kog uređaja glutopika u proceni kvaliteta bra&scaron;na i finalnog proizvoda &ndash; hleba, kao i mogućnost zamene tradicionalnih dugotrajnih metoda novom reolo&scaron;kom metodom.<br />Kako bi se ispitale i iskoristile mogućnosti reolo&scaron;kog uređaja glutopik za procenu kvaliteta p&scaron;eničnog bra&scaron;na definisani su optimalni uslovi merenja koji su podrazumevali upotrebu NaCl kao rastvarača i zadate parametre temperature (36 &deg;C), obrtne brzine me&scaron;ača (2700 rpm) i odnos bra&scaron;na i rastvarača (8,5/9,5). Zabeležen je veliki broj korelacija između parametara glutopika i empirijskih reolo&scaron;kih pokazatelja kvaliteta bra&scaron;na i testa. Takođe je utvrđena značajna korelacija između parametara glutopika i indikatora kvaliteta hleba u pogledu specifične zapremine i teksturnih karakteristika sredine hleba. Na osnovu parametara dobijenih merenjem na glutopiku definisane su granične vrednosti. Ustanovljeno je da se primenom glutopik metode može izvr&scaron;iti klasifikacija sorti p&scaron;enice prema kvalitetu. Pored toga, utvrđeno je da glutopik ima veliki potencijal da zameni alveograf u proceni kvaliteta bra&scaron;na u mlinarskoj i pekarskoj industriji. Reolo&scaron;ki parametri koji zavise od sadržaja proteina kao &scaron;to su moć upijanja vode i žilavost testa uspe&scaron;no se mogu predvideti pomoću parametara glutopika. Primenom glutopik metode postignuta je umerena predikcija specifične zapremine hleba, dok je postignuta veoma dobra predikcija teksturnih karakteristika sredine hleba.<br />U okviru ove disertacije je ispitan uticaj sorte i lokaliteta na tehnolo&scaron;ki kvalitet bra&scaron;na p&scaron;enice kako bi se utvrdilo koja od ispitivanih sorti ispoljava ujednačen kvalitet u različitim mikroklimatskim uslovima tokom dve proizvodne godine. U obe proizvodne godine pokazatelji kvaliteta bra&scaron;na su dominantno sortno određeni, pri čemu je zabeležen određeni uticaj mikroklimatskih faktora na lokalitetima gajenja. Odličan i najstabilniji kvalitet bra&scaron;na u 2011. godini je imala sorta Gordana koja je pokazala najveću adaptabilnost na mikroklimatske uslove. Apač je uniformno imao najlo&scaron;iji kvalitet duž svih ispitivanih lokaliteta. Domaće sorte su u 2012. godini imale promenljiv kvalitet u zavisnosti od lokaliteta gajenja. Hlebove proizvedene od domaćih p&scaron;eničnih sorti je karakterisala velika zapremina, rastresita struktura sredine sa izraženim velikim porama i mala čvrstoća sredine, dok je hleb proizveden od sorte Apač imao malu zapreminu, zbijenu strukturu sredine hleba sa velikim brojem malih pora kao posledicu velike čvrstoće. Dobra predikcija kvaliteta hleba od bra&scaron;na iz 2011. godine je postignuta primenom jednog reolo&scaron;kog pokazatelja kvaliteta, dok je za uspe&scaron;nu predikciju kvaliteta hleba od bra&scaron;na iz 2012. godine neophodno izvesti nekoliko različitih reolo&scaron;kih merenja.<br />Analizom tehnolo&scaron;kog kvaliteta bra&scaron;na p&scaron;enice različitih sorti gajenih na različitim lokalitetima iz tri proizvodne godine zabeležene su velike varijacije u kvalitetu bra&scaron;na i hleba na ispitivanim lokalitetima i u proizvodnim godinama, &scaron;to jasno ukazuje na značajan uticaj interakcija između sortimenta i uslova gajenja (lokaliteta i godina), kao i značaj ispitivanja ovih interakcija i razvoja strategija koje imaju za cilj smanjenje uticaja spolja&scaron;njih faktora na kvalitet p&scaron;enice.</p> / <p>Regardless the fact that numerous traditional rheological methods have been used for many years in the flour quality assessment, there is a need for developing new methods, which could, in a short time, and with a limited amount of sample, successfully predict the quality of flour and finished products. In this way, wheat breeders would be able to evaluate the technological quality of the wheat lines with a restricted sample quantity, while the millers would be provided with a quick method of the quality evaluation. The main goal of the research of this dissertation was to examine the possibility of using a new rheological device GlutoPeak in the quality evaluation of flour and final product &ndash; bread, as well as the possibility of replacing traditional time-consuming methods with a new rheological test.<br />In order to examine the possibility of using a GlutoPeak rheological device for the flour quality evaluation, the optimal measurement conditions were defined and included the use of NaCl as a solvent, the rotational speed of the mixer (2700 rpm), temperature (36 &deg;C), the ratio of flour and solvent (8.5/9.5). Numerous correlations between GlutoPeak indices and empirical rheological parameters of dough behaviour were reported in this study. Significant correations were also observed between GlutoPeak parameters and bread specific volume and breadcrumb textural properties. The limit values were defined according to the GlutoPeak parameters values. Moreover, it was found that the GlutoPeak test could be used for wheat variety diferentiation according to the quality and has a great potential to replace Alveograph in the flour quality assessment in the milling and bakery industries. Parameters which depends on the protein content, such as, flour water absorption and dough tenacity, was successfully predicted by using parameters derived from GlutoPeak tester. A moderate prediction of loaf specific volume was achieved, while a very good prediction of breadcrumb textural characteristics was accomplished with the GlutoPeak parameters.<br />In addition, the influence of genotype and growing location on flour quality was examined in order to determine which of the tested varieties exhibited uniform quality accross different microclimatic conditions in two production years. It was revealed that in both production years flour quality indicators were predominantly influenced by genotype, with a certain influence of microclimate factors on the growing locations. Gordana variety showed excellent and uniform quality with the highest adaptability to microclimate conditions in year 2011. Apache variety showed uniformly poor quality across all tested locations. In year 2012 domestic varieties exhibited variable quality depending on the growing locations. Bread produced from domestic wheat varieties was characterized by a large volume, loose breadcrumb structure with pronounced large pores and low hardness, while the bread produced from Apache variety had a small volume, dense breadcrumb structure with a large number of small pores as a result of high breadcrumb hardness. The quality of bread produced from wheat flour from year 2011 was well predicted based on one rheological quality parameter. On the other hand, several different rheological measurements was performed to successfully predict the quality of bread produced from wheat flour from 2012 year.<br />By analyzing the technological quality of wheat flour of different varieties cultivated at different locations from three production years, large variations in the quality of flour and bread was recorded. The variations in flour and bread quality indicated the significant influence of interactions between the variety and growing conditions (locations and years), as well as the importance of examining these interactions and developing strategies aimed at reducing the impact of external factors on wheat quality.</p>

Neste trabalho nanocompósitos de copolímero em bloco foram estudados. Os copolímeros em bloco utilizados foram o SEBS (poliestireno-b-poli(etileno-co-butileno)-b-poliestireno) e SEBSMA (que contém cerca de 2% de anidrido maléico no bloco de PEB) e as nanocargas argilas organofílicas: Cloisite 20A (modificada com 95 meg/100g de argila do sal di(alquil de sebo hidrogenado) dimetil amônio) e Cloisite 30B (modificada com 90 meq/100g de argila do sal (alquil de sebo) dihidroxietil metil amônio). Os nanocompósitos foram obtidos pelo método de mistura no estado fundido utilizando uma extrusora dupla rosca. Foram utilizados dois tipos de matrizes, sendo uma de filamento e a outra de fita. As microestruturas e propriedades dos materiais resultantes foram caracterizadas pelas técnicas de Espalhamento de Raios X a Baixo Ângulo (SAXS), Difração de Raios X (XRD), Microscopia Eletrônica de Transmissão (TEM). Foram realizados ensaios de Cisalhamento Oscilatório em Pequenas Amplitudes (SAOS) e Varredura de tempo (Time Sweep). Também, foram realizadas séries de ensaios reológicos para estudar um possível alinhamento das estruturas durante o fluxo. Em particular as amostras foram submetidas a Cisalhamento Oscilatório em Grandes Amplitudes (LAOS) e a estabilidade estrutural do material após o alinhamento. As amostras foram também testadas em fluxos extensionais utilizando-se uma geometria apropriada para gerar fluxos elongacionais. Esses últimos ensaios foram realizados utilizando dois tipos de amostras: amostras obtidas com a matriz de fita e cortadas paralelamente à direção do fluxo (longitudinal) ou perpendicularmente a direção do fluxo (transversal). As análises de caracterização estrutural (XRD e TEM) indicaram uma estrutura intercalada para o nanocompósito SEBS/20A, esfoliada para o SEBS-MA/20A e parcialmente esfoliada para o nanocompósito SEBS-MA/30B. Os resultados mostraram que as estruturas estão bem ordenadas com empacotamento hexagonal cilíndrico para ambos os copolímeros e nanocompósitos. Os resultados de caracterização estrutural mostraram que o processo de extrusão alinhou os cilindros (PS) na direção do fluxo de extrusão e as partículas de argila também sofreram uma orientação preferencial em menor escala. A caracterização reológica das amostras em cisalhamento mostrou que as morfologias dos nanocompósitos são estáveis com o tempo de cisalhamento, e permitiu confirmar as morfologias dos nanocompósitos. Os ensaios reológicos mostraram que é possível orientar as morfologias em cisalhamento e extensão. / In this work nanocomposites block copolymer were studied. The block copolymers used were SEBS (polystyrene-b-poly(ethylene-co-butylene)-b-polystyrene) and SEBS-MA (containing about 2% of maleic anhydride in the block EB), the nanocharges were organoclays namely: Cloisite 20A (modified with 95 meg/100g clay salt di (hydrogenated tallow alkyl) dimethyl ammonium) and Cloisite 30B (modified with 90 meq/100 g clay salt (tallow alkyl) methyl ammonium dihidroxietil). The nanocomposites were obtained by melt mixing using a twin-screw extruder. Two types of matrices, filament and ribbon were used. The microstructures and properties of the resulting materials were characterized by Small Angle X-Ray Scattering (SAXS), X-Ray Diffraction (XRD) and Transmission Electron Microscopy (TEM). Small Amplitude Oscillatory Shear (SAOS) and Time Sweep were carried out. Sequences of rheological tests were conducted to study a possible alignment of the structures during flow. In particular, the samples were submitted to Large Amplitude Oscillatory Shear (LAOS) and recovery. The samples were also tested in extensional flows using an appropriate geometry. These latest tests were conducted using two types of samples: tape samples cut along the flow direction (longitudinal) or cut perpendicular to the flow direction (transverse). The analysis of structural characterization (XRD and TEM) indicated an intercaled structure of the nanocomposite SEBS/20A, exfoliated for SEBS-MA/20A and partially exfoliated nanocomposite for SEBS-MA/30B. The results showed that the structures are well ordered with hexagonal cylindrical packing for both copolymers and nanocomposites. The results of structural characterization showed that the extrusion process aligned cylinders (PS) in the flow direction of extrusion and the clay particles also suffered a preferred orientation on a smaller scale. The rheological characterization of the samples in shear showed that the morphologies of the nanocomposites are stable with time of shearing, and it confirmed the morphologies of the nanocomposites. The rheological tests showed that it is possible to guide the morphologies in shear and extension.

O tema deste trabalho é o estudo de métodos numéricos para a simulação de escoamentos incompressíveis com superfície livre a baixos Reynolds, por meio da metodologia GENSMAC e suas formulações explícita e implícita. Neste contexto, temos especial interesse na formulação implícita, objetivando o enfraquecimento da restrição de estabilidade parabólica no passo temporal em escoamentos com superfície livre. O trabalho pode ser dividido em duas partes: na primeira, algumas modificações são discutidas, propostas e testadas com o objetivo de tornar a formulação implícita mais eficiente e precisa; em seguida, aproveitamos os resultados obtidos e generalizamos o método numérico existente para simular escoamentos viscoelásticos modelados pela equação constitutiva SXPP. Em ambos os casos, a formulação explícita também é usada para comparação e teste. Resultados que demonstram a eficiência e robustez das técnicas desenvolvidas são apresentados por meio da simulação numérica de complexos problemas envolvendo superfície livre.O tema deste trabalho é o estudo de métodos numéricos para a simulação de escoamentos incom- pressíveis com superfície livre a baixos Reynolds, por meio da metodologia GENSMAC e suas formulações explícita e implícita. Neste contexto, temos especial interesse na formulação implícita, objetivando o en- fraquecimento da restrição de estabilidade parabólica no passo temporal em escoamentos com superfície livre. O trabalho pode ser dividido em duas partes: na primeira, algumas modificações são discutidas, propostas e testadas com o objetivo de tornar a formulação implícita mais eficiente e precisa; em seguida, aproveitamos os resultados obtidos e generalizamos o método numérico existente para simular escoamentos viscoelásticos modelados pela equação constitutiva SXPP. Em ambos os casos, a formulação explícita também é usada para comparação e teste. Resultados que demonstram a eficiência e robustez das técnicas desenvolvidas são apresentados por meio da simulação numérica de complexos problemas envolvendo superfície livre / The purpose of this work is the study of numerical methods for low Reynolds number incompressible free surface flows, including the GENSMAC methodology and its explicit and implicit formulations. In this context, we have special interest in the implicit formulation, in order to circumvent the parabolic stability restriction in the time step for free surface flows. The work can be divided into two parts: firstly, some modifications are proposed, discussed, and tested with the purpose of making the implicit formulation more e¢ cient and accurate; secondly, we take advantage of the results derived in the first part to generalize the numerical method for simulating viscoelastic free surface flows modeled by the constitutive equation SXPP. In both cases, the explicit formulation is also used for comparison and tests. Results that demonstrate the e¢ ciency and robustness of the developed techniques are presented and illustrated by the numerical simulation of complex problems involving free surface flows

Todos os seres vivos compartilham uma característica comum na sua composição estrutural, a célula. No corpo humano, as células vasculares de músculo liso são fundamentais para o bom funcionamento dos vasos arteriais. A principal função dessas células é contrair e regular o calibre desses vasos, a pressão sanguínea e a distribuição do fluxo de sangue. Devido a isto, alterações mecânicas sofridas por estas células acarretam modificações estruturais nos vasos, podendo levar à hipertensão, vasoespasmo e arteriosclerose. O principal objetivo do nosso trabalho foi o de desenvolver uma nova plataforma de análise de imagens de células vasculares para caracterizar suas propriedades estruturais. Em nossa plataforma, analisamos parâmetros estruturais de células vasculares de músculo liso de diferentes leitos arteriais, com as fibras de actina evidenciadas com marcadores fluorescentes, obtidas por microscopia confocal. Estes parâmetros são: o Índice de Alinhamento das fibras de actina da imagem, a distribuição de comprimento dessas fibras e sua dimensão fractal. Mostramos que com esses parâmetros somos capazes de comparar células de leitos arteriais diferentes de forma quantitativa, assim como, correlacionar esses parâmetros com suas propriedades mecânicas. / All living organisms share a unique characteristic in their structural composition, the cell. In the human body, vascular smooth muscle cells are fundamental for the ideal functioning of the arterial vessels. The main function of these cells is to contract and regulate these vessels caliber, as well as the blood pressure and flow distribution of blood. Due to the exposed above, mechanical alterations suffered by these cells cause structural modifications in vessels, which may lead to hypertension, vasospasm and atherosclerosis. The main objective of our research was to develop a new framework of image analysis for vessel cells in order to characterize their structural properties. In our framework we analyzed structural parameters of vascular smooth muscle cells from different arterial sites, with actin fibers labeled with fluorescent markers, obtained by confocal microscopy. These parameters are: the actin fibers alignment index of the image, the length distribution of these fibers and their fractal dimension. We presented that with these parameters we are able to quantitatively compare cells in different arterial sites as well as correlate these parameters with their mechanical properties.

L'argile est utilisée avec des polymères en solution dans de nombreuses applications telles que les boues de forage ou encore pour rendre les fibres textiles résistantes au feu. Du fait de la structure très particulière des particules d'argile, avec plusieurs échelles d'association de feuillets, les propriétés rhéologiques de dispersions d'argile dans des solutions de polymère dépendent fortement de l'histoire mécanique du matériau. Une étude de vieillissement des dispersions d'argile dans les solutions aqueuses de CMC a montré l'effet du temps, en particulier sur l'existence d'un seuil de contrainte et son évolution. Les mesures rhéologiques mettent en évidence des comportements de type « gel ». Ils résultent de la formation, au sein du fluide, de réseaux élastiques de nature différente selon la phase continue utilisée. Dans l'eau, les particules partiellement exfoliées s'associent entre elles selon des mécanismes qui dépendent du pH. Alors que dans la solution de polymère, il semble que des agrégats de particules soient connectés entre eux par l'intermédiaire des chaînes macromoléculaires. L'influence de la température et du pH sur les propriétés rhéologiques a été examinée. Plusieurs expériences indépendantes ont montré une évolution non monotone des caractéristiques mécaniques des fluides lorsque la température augmente. Ceci peut s'expliquer en invoquant un accroissement de la mobilité des chaînes favorisant l'ouverture des agrégats se dissociant en agrégats de plus petite taille. Le contrôle du pH quant à lui permet de modifier les interactions particule-particule et particule-polymère et, de ce fait, d'agir sur les propriétés mécaniques des gels formés. / The clay is used with polymer solutions in numerous applications such as drilling muds or to make textile fibers fireproof. Because of the very particular structure of the clay particles, with several scales of association of platelets, the rheological properties of clay dispersions in aqueous polymer solutions strongly depend on the mechanical history of the material. An ageing study of clay dispersion in aqueous CMC solutions showed the effect of time, in particular on the existence of a yield stress and its evolution. The rheological measurements display gel like behaviours. They are the result of formation, within the fluid, of different kind of networks, depending on the continuous phase. The partially exfoliated particles join together according to mechanisms which depend on the pH. While in the polymer solution, it seems that particle aggregates are connected through the macromolecular chains. The influence of the temperature and the pH on the rheological properties is studied. Several independent experiments show a non-monotonous evolution of the mechanical properties of the fluids as the temperature increases. It may be due to an increase of the mobility of the macromolecular chains favouring the dissociation of the particles aggregates. The control of the pH allows the particle-particle and particle-polymer interactions to be modified and to therefore act on the mechanical properties of the gels.

<p>Stabilizatori na bazi biopolimera postaju posebno povoljna prirodna re&scaron;enja za primenu u kompleksnim sistemima, kao &scaron;to su emulzije tipa ulja u vodi. U ovoj disertaciji je ispitan individualni i kombinovani uticaj tri stabilizatora na bazi polisaharida (vlakna &scaron;ećerne repe, pektin &scaron;ećerne repe i OSA maltodekstrin) na formiranje i stabilnost emulzija kukuruznog ulja u vodi. Ispitan je uticaj četiri različite tehnike emulgovanja (ultrazvučna homogenizacija, visokopritisna homogenizacija, membransko emulgovanje i rotor-stator homogenizacija). Sveobuhvatna karakterizacija koja je obuhvatala ispitivanje fizičko-hemijskih, strukturnih, tenziometrijskih, konduktometrijskih, viskozimetrijskih osobina ispitivanih polisaharida je prikazana u ovoj disertaciji. Dobijeni rezultati veličine kapi emulzija i njihove fizičke stabilnosti ukazuju na dobra stabilizaciona svojstva ispitivanih polisaharida. Interakcije između primenjenih stabilizatora na bazi polisaharida rezultovale su značajnim promenama veličine kapi, zeta potencijala, kriming indeksa i strukture emulzije.</p> / <p>Biopolymer based stabilizers become particularly favorable natural solutions for use in complex systems, such as oil-in-water emulsions. In following dissertation, the individual and combined effects of three polysaccharide based stabilizers (sugar beet fibers, sugar beet pectin and OSA maltodextrin) on the formation and stability of corn oil emulsions in water were tested. The influence of four different emulsion techniques (ultrasonic homogenization, high-pressure homogenization, membrane emulsification and rotor-stator homogenization) were examined. A comprehensive characterization that included the examination of physico-chemical, structural, tensiometric, conductometric, viscometric characteristics of the polysaccharides examined is presented in this dissertation. The obtained results of the emulsion droplet size and their physical stability indicate good stabilization properties of the polysaccharides examined. The interactions between the applied polysaccharide-based stabilizers resulted in significant changes in the droplet size, zeta potential, creaming index and the structure of the emulsion.</p>

Depuis plus de 20 ans, de nombreuses méthodes et techniques non invasives ont été développées en vue de mesurer le plus objectivement possible, les propriétés (physico-chimiques, sensorielles, etc.) des produits cosmétiques. Ces méthodes visent à évaluer leur innocuité et leur efficacité, et deviennent d’autant plus perfectionnées que les processus d’élaborations de ces produits deviennent complexes et innovants.Au cours de ces travaux de thèse, une étude multi-échelle, de l'évolution structurale d'émulsions cosmétiques représentatives des crèmes mises sur le marché a été menée, afin de prédire leur stabilité tant texturale que microbiologique.L’étude du lien entre l’organisation structurale de ces émulsions avec leur composition et leur stabilité a été un des premiers défis à relever. Grâce à une technique non destructive ultrasonore permettant d’accéder aux propriétés micro-rhéologiques (propriétés viscoélastiques observée lors d'une sollicitation harmonique de cisaillement à quelques MHz), en association à différentes techniques classiques de caractérisation (microscopie optique, rhéologie basse fréquence, etc.) ; il a été possible de corréler les paramètres micro-rhéologiques obtenus à des modèles physiques reliant structuration interne et stabilité dans les émulsions considérées. Les résultats ont montrés que les données micro-rhéologiques sont sensibles aux variations de compositions (concentration) et d’organisations microscopiques des micelles au sein des émulsions (floculation, coalescence, etc.).Ensuite, le suivi de l’évolution d’une bactérie type (Pseudomonas fluorescens) dans des émulsions possédant des structures internes différentes, a montré d’une part la sensibilité de la micro-rhéologie vis-à-vis de la présence de bactéries dans le milieu, et d’autre part, l’impact de la structure et l’organisation des micelles sur le développement de ces bactéries.Finalement, la micro-rhéologie apparait être une méthode de mesure innovante et adaptée à l’échelle industrielle apportant une valeur ajoutée lors du développement de formulations cosmétiques. D’un point de vue sécuritaire, le dépistage précoce de contaminations biologiques par la détection d’instabilités (de changements) structurales au sein des émulsions, pourrait représenter une avancée majeure lors des phases de production et de commercialisation des produits cosmétiques. / In the last 20 years, many non-invasive methods and techniques have been developed in order to measure the properties (physicochemical, sensory, etc.) of cosmetic products. These methods are designed to evaluate their safety and effectiveness, and become even more sophisticated as the processes of developing these products become complex and innovative.During this thesis works, a multi-scale study of the structural evolution of cosmetic emulsions was conducted in order to predict their textural and microbiological stability.The study of the link between the structural organization of these emulsions with their composition and their stability was one of the first challenges. Thanks to an ultrasonic non-destructive technique allowing access to micro-rheological properties (viscoelastic properties observed during a harmonic loading of shear at a few MHz), in association with different classical characterization techniques (optical microscopy, low frequency rheology, etc. .); it was possible to correlate the micro-rheological parameters obtained with physical models linking internal structuring and stability in the emulsions considered. The results showed that micro-rheological data are sensitive to variations in compositions (concentration) and microscopic organization of micelles within emulsions (flocculation, coalescence, etc.).Then, the follow-up of the evolution of Pseudomonas fluorescens bacteria in emulsions with different internal structures showed on the one hand the sensitivity of micro-rheology towards the presence of bacteria in the cream, and on the other hand, the impact of the structure and organization of micelles on the development of these bacteria.Finally, micro-rheology appears to be an innovative measurement method adapted on an industrial scale providing added value when developing cosmetic formulations. From a safety point of view, the early detection of biological contaminations by the detection of structural instabilities (of changes) within emulsions could represent a major advance during the production and marketing phases of cosmetic products.

The properties of the aged gel and subsequent softgels were examined using mechanical and chemical testing methods. Our hypothesis was that a negligible variation will exist between the aged gel of the same type. The greater difference is expected to be seen between the types of gels described as 150 Bloom (alkaline treated collagen) and 195 Bloom (acid treated collagen). The types of gelatin used were the acid processed (195 Acid Bone) and alkaline processed (150 Lime Bone). Because of the differences expressed as the result of their manufacture sequence (namely their molecular weights), it follows that physical attributes will further contribute to their distinction. In addition to observing different characteristics between the types of gels, we aged the gelatin and produced softgel capsules to qualify and quantify the changes that occur as a function of time. Two production lots of over 1 million softgel capsules were executed to produce a population that lends itself to statistical analysis. Softgel capsules were manufactured with gelatin which was aged at intervals of 0-8 hrs, 32-40 hrs, 66-72 hrs and 88-96 hrs. The manufacturing process made use of this strategy for the acid and alkaline treated gelatin where a total of eight lots were made (4 acid and 4 alkaline). One hundred thousand softgels were manufactured for the acid processed gelatin, per lot. Additionally, one hundred and fifty thousand softgels were manufactured for the alkaline processed gelatin per lot. The results of the different tests provided trends that were not solely a function of time. Gel extensibility for both gel types showed a decrease in the amount of force needed to rupture the gelatin ribbon, as a function of time. The resilience of the tested ribbon remained constant throughout the aging process. The burst strength was the only test showing an inverse relationship between the two gel types. The amount of force needed to rupture the 150 Bloom softgels decrease in time whereas the amount of force needed to rupture the 195 Bloom softgels increase with time. The rheological testing was described in the literature as being associated with the molecular weight distribution. Such association was seen in our research and both the results of the rheological and the molecular weight tests decreased with the aging process.

Le rhéoépaississement est un phénomène spectaculaire apparaissant dans certaines suspensions concentrées en particules. Il se manifeste par l’augmentation brutale de la viscosité de la suspension au delà d’une contrainte critique. L’exemple emblématique de suspension présentant ce type de comportement est le mélange d’amidon de maïs et d’eau. Le rhéoépaississement est longtemps resté une énigme, jusqu’à des travaux théoriques et numériques récents proposant un modèle microscopique cohérent. Selon celui-ci, le rhéoépaississement provient d’une transition frictionnelle due à la présence d’une force répulsive entre les grains. Au cours de ma thèse, j’ai réalisé une des premières démonstrations expérimentales directe de ce mécanisme. En m'inspirant de travaux venant du domaine des milieux granulaires, j'ai montré qu'en accord avec le modèle de transition frictionnelle, une suspension rhéoépaississante possède à faible pression granulaire un état non frottant. J'ai ensuite mis en évidence la transition en elle-même dans des suspensions contrôlées de billes de silice dans des solutions salines. Pour cela, j'ai dû développer de nouvelles méthodes de rhéologie à pression imposée. En effet, les rhéomètres standard ne permettent pas d'accéder aux propriétés de frottement des suspensions. Le seul rhéomètre qui le permet n'est pas adapté aux suspensions étudiées ici, qui sont constituées de particules colloïdales. Ce travail ouvre donc la voie au développement d’une nouvelle génération de rhéomètres permettant de mesurer le frottement dans les suspensions colloïdales, un enjeu majeur pour la rhéologie des fluides complexes. / Shear thickening is a spectacular phenomenon which takes place in some dense suspensions. It manifests itself by a brutal increase of the suspension's viscosity above a certain critical stress. The most iconic example of shear-thickening suspensions is cornstarch and water mixes. Shear thickening long remained a mystery, until recent theoretical and numerical works which proposed a consistent microscopic model. This model explains the shear thickening transition as a frictional one due to the presence of a repulsive force between the grains.During my PhD, I provided one of the first direct experimental proofs of this mechanism. Inspired by granular physics, I showed that shear-thickening suspensions possess a frictionless flowing state at low granular pressure, which is consistent with the proposed model. I then evidenced the frictional transition with controlled experiments using suspensions of silica beads in ionic solutions. To do this, I developed new rheological techniques enabling pressure imposed measurements. Indeed, standard rheological tools do not allow access to the frictional properties of suspensions. The only rheometer that does that is not adapted to the suspensions we study here, which are colloidal. This work thus paves the way for the development of a new generation of pressure imposed rheometers, giving access to colloidal suspensions friction, which is a major challenge in complex fluids rheology.