On s'intéresse dans le présent travail au comportement au gel des sols fins limono-argileux traités à la chaux seule, sols valorisables qui sont couramment rencontrés sur les chantiers de terrassement. Trois sols appartenant aux classifications A1, A2, A3 selon la norme NF P 11300, ont été choisis pour cette étude. Ces sols sont traités à 3 dosages en chaux correspondant à 3 objectifs : 1) amélioration (dosage en chaux minimal), 2) stabilisation et insensibilité à l'eau (dosage en chaux intermédiaire), 3) stabilisation et résistance au gel (dosage en chaux le plus élevé). Les sols traités sont ensuite conservés pendant quatre périodes de cure : 7 jours, 28 jours, 90 jours et 365 jours. Les deux processus de gel - le géligonflement et la gélifraction sont étudiés, parallèlement à l'évaluation des performances mécaniques, hydrauliques et microstructurales. Les résultats expérimentaux ont montré que les propriétés hydrauliques (la succion au front de gel, sp et la conductivité hydraulique à l'état non-saturé, kunsat) sont les paramètres qui gouvernent le phénomène de géligonflement des sols, traités ou non. Les résultats ont également mis en évidence le lien direct existant entre la microstructure (la distribution porale) et les propriétés hydrauliques du sol, principalement en termes de capacité de rétention d'eau et conductivité hydraulique. Le traitement augmente les performances mécaniques des sols d'une part, et amène d'autre part à des modifications de leur microstructure ; ceci induit des changements vis-à-vis de leur sensibilité au gel. Les sols sont plus gélifs directement après le traitement, cette sensibilité au gel diminuant avec le temps de cure. Une modélisation simple permettant d'estimer le gonflement au gel à partir de la succion au front de gel et de la valeur de conductivité hydraulique à l'état non-saturé a été proposée et validée. Vu que la détermination de la conductivité hydraulique à l'état non-saturé n'est pas un essai couramment pratiqué au sein de la plupart des laboratoires, un critère basé sur la succion au front de gel, sp, et la conductivité hydraulique à l'état saturé, ksat a été proposé pour évaluer la sensibilité des sols au gel. L'essai de gélifraction consiste à évaluer un coefficient de résistance de l'éprouvette de sol après 10 cycles de gel/dégel, RFT (%) - « retained strength factor after freeze-thaw testing ». Les résultats expérimentaux montrent que la valeur RFT des sols traités varie de 0% (lorsque les éprouvettes de sol perdent totalement leur résistance à la compression simple et sont détruites après 10 cycles de gel/dégel) à 90%. Quand RFT ≥ 60%, aucune dégradation visuelle de la surface des éprouvettes des sols traités n'est constatée. Ainsi, cette valeur est proposée comme critère d'acceptation des matériaux constitutifs d'une couche de forme subissant le gel avant son recouvrement. L'étude de l'effet du nombre des cycles de gel/dégel montre une diminution importante de la performance mécanique (RFT) durant trois premiers cycles de gel/dégel, et ce paramètre se stabilisant après 10 cycles. A l'aide de la technique de µ Tomographie X, l'endommagement interne des éprouvettes de sol ayant subi des cycles de gel/dégel a été quantifié. Une corrélation directe entre la diminution de performance mécanique et l'augmentation de l'indice de l'endommagement de l'éprouvette a été mise en évidence. Enfin, un modèle d'endommagement permettant d'évaluer la dégradation de la performance mécanique avec l'augmentation de l'indice d'endommagement a été établi / The present work deals with the behaviour of fine-grained silty and clayey soils treated with lime under frost. Those soils are frequently encountered in earthworks. Three soils corresponding to A1, A2, A3 classes according French NF P 11-300 standard were chosen for this study. These soils were treated with 3 lime dosages corresponding to three objectives: 1) improvement (minimum dosage), 2) stabilization and insensitivity to water (intermediate dosage), 3) stabilization and frost resistance (highest dosage). Lime-treated soils were subsequently cured for different times: 7, 28, 90, 365 days. Two frost processes, frost heave and freeze-thaw cycles, were applied in parallel with the assessment of mechanical, hydraulic and microstructural properties. Experimental results evidenced that it is the hydraulic properties (suction at frost front, sp and unsaturated hydraulic conductivity, kunsat) that govern the frost heave phenomenon of soils, treated or not. In addition, this study demonstrates the direct link between the microstructure (the pore size distribution) and the hydraulic properties (water retention curve and hydraulic conductivity). The treatment on one hand improves the mechanical performances of soils, and on the other hand modify their microstructure, and thus changes their frost sensitivity. The frost susceptibility increases directly after treatment, and then decreases with curing time. Based on the suction at frost front and the unsaturated hydraulic conductivity, a simple model was proposed and validated allowing to estimate the frost heave. Considering that the determination of unsaturated hydraulic conductivity is not a test commonly performed by most laboratories, a criterion based on the suction at frost front and the saturated hydraulic conductivity was proposed to estimate the frost sensibility of soils. The second frost resistance test consists of measuring the retained strength factor after 10 freeze-thaw cycles, RFT (%). The results obtained show that RFT of lime treated soil varies from 0% (when soil specimen completely loses its resistance and collapses after 10 freezethaw cycles) to 90%. When RFT is higher than 60%, no visual damage was observed on the specimen surface; consequently, this value is proposed as a criterion for acceptance of lime treated soil in capping layer before covering. In addition, the study of effect of freeze-thaw cycles showed a significant decrease of mechanical performance (RFT) during the first three cycles, and a stabilization after 10 cycles. Using X-ray Tomography, the intern damage of specimens due to freeze-thaw cycles was quantified. A correlation between the decrease of mechanical performance and the increase of damage index was evidenced. A model was then developed to evaluate the degradation of mechanical performance with the increase of damage index

0 comportamento higroscópico do suco de laranja liofilizado, e aditivado com malto-dextrinas e lactose, e de misturas mecânicas do suco liofilizado com os aditivos secos, foi estudado através da cinética e das isotermas de sorção de água, em diferentes temperaturas. Avaliou-se as características espectrais no visível e ultravioleta, e o teor de vitamina C, de amostras de suco de laranja liofilizado expostas a diferentes umidades relativas e temperaturas. Estudou-se a influência do valor de pH e natureza do tampão sobre a retenção do limoneno emulsionado em soluções de lactose, liofilizadas. A liofilização praticamente não alterou o teor de vitamina C e as características espectrais do suco de laranja, mas aumentou o valor monomolecular da malto-dextrina (dextrose equivalente de 9 a 12%). A lactose liofilizada apresentou-se no estado amorfo. Os teores de umidade de equilíbrio das misturas aditivadas liofilizadas, foram menores que os das misturas mecânicas. Os aditivos reduziram a sorção de umidade em função do tempo. A retenção do limoneno foi influenciada pela sua concentração inicial, sendo que ocorreu a major perda, durante a liofilização na major concentração utilizada. / The higroscopic behavior of freeze-dried orange juice, with added maltodextrins and lactose and mechanical mixtures with this additives was studied through the kinetics and isoterms of water sorption in different temperatures. It was evaluated the spectral characteristics, in the visible and ultraviolet range, and the vitamin C content from samples of freeze-dried orange juice exposed at different relative humidities and temperatures. It was studied the influence of pH and buffer composition, on the limonene retention of freeze-dried emulsions. The spectral characteristics and vitamin C content showed no alterations after liofilization the maltodextrin (9-12 % dextrose equivalent monomolecular value increased. Freezedried lactose was amorphous. The equilibrium humidity content of the samples with additives were reduced when compared with mechanical mixtures. The additives also reduced the rate of water sorption. The limonene retention during freeze-drying was influenced by the initial concentration of the emulsion. The greater concentration studied showed the lower retention value.

This diploma thesis describes research and following development of lightweight cement mortars with alternative raw materials. Attention was focused on study of the effects of extreme influences such as high temperature (up to 1200 °C), freeze-thaw and agressive sulfur dioxide. Verification of durability of developed mortars was realized using physical and mechanical tests (density and strength), physical and chemical methods (computed tomography) and scanning electron microscopy. Assessment of durability was realized in a longer period of time (90 days).

The diploma thesis deals with different methods of determining levels of degradation of concrete due to freezing, also considering the options of freeze thaw resistance determination in structure. At first the properties of concrete and possible mechanisms of concrete degradation are described – mainly the effects of freezing water in the inner structure and of the combination of freezing water and de-icing chemicals on the surface. Principle and properties of air-entrained concrete are also mentioned. An overview of the approaches that current standards use to determine the freeze-thaw resistance of concrete is listed, followed by description of the tests that are used on air-entrained concrete specimens in the main part of the thesis. A portion of the test specimens was made in moulds while the rest was obtained from structure (concrete block). The non-destructive tests used are evaluated in several different ways and their results are compared with the destructive tests. Comparison and evaluation of different approaches used to determine the freeze-thaw resistence of concrete are the main outcome of this thesis.

Hyaluronan is a chemical, which can be qualified as essential for vertebrates. It is a part of the extracellular matrix in most of tissues and also a major component of some other tissues. Besides of the mechanical functions this compound is important for many biological processes such as growth of tumor cells. The objective of this thesis was development of carrier systems containing native hyaluronan and hydrophobic drugs. For purposes of this work fluorescence probes (pyrene, prodan, perylene, DPH, mereocynine 540) instead of drugs were used. By using further mentioned sophisticated methods the properties of these systems were studied. The systems were prepared by freeze-drying. The effect of freeze-drying on support of interactions was observed by fluorescence spectrometry (steady-state and time-resolved). The stability of freeze-dried systems was determined by zeta potential, which was measured by electrophoretic light scattering. Cakes obtained by freeze-drying were analyzed by several methods. First one was effluence gas chromatography connected with FT-IR spectrometry. In this method the present of tertiary butyl alcohol in product was observed. The cakes were also analyzed by scanning electron microscopy, which can provide the information about the surface and elemental constitution of the material. The results of this work can shed light on the area of developing of drugs with targeted distribution of active compound.

This thesis describes the convenient routes and the preparation conditions (temperature, oxygen partial presssure) which lead to the formation of single phase materials within the quaternary system Cu-Ni-Fe-O. The investigated compositions are the solid solutions CuxNi1-xFe2O4, the ferrites occurring in the phase triangle Cu0.5Ni0.5Fe2O4 -Cu0.9Fe2.1O4 - Cu0.5Fe2.5O4 and some copper-nickel oxide solid solutions. Three synthesis routes have been used, namely (i) the preparation and the thermal decomposition of freeze-dried carboxylate precursors, (ii) the preparation and the oxidation of intermetallic phases and (iii) the preparation and the heat treatment in air of mixed oxide/metallic powders. The thermal decomposition of freeze-dried Cu-Ni-Fe formate has been found as a suitable method for preparing single spinel phases within the Cu-Ni-Fe-O system. In comparison with the conventional solid state reaction, the required temperature is much lower. Concerning the solid solution CuxNi1-xFe2O4 , a single phase spinel is formed at 1000¢XC for x < 0.7; for CuO is identified as second phase. In this latter range the formation of a pure phase required an increase of the iron content in the mixture. The other single spinel phases in the phase triangle Cu0.5Ni0.5Fe2O4 - Cu0.9Fe2.1O4 - Cu0.5Fe2.5O4 have been synthesized under special synthesis p(O2)/T-conditions. For copper ferrites Cu1-xFe2+xO4 with x ?­ 0.1, 0.2, 0.33, 0.4 and 0.5, the change in the conductivity with the temperature is irreversible. The deviation from the linearity of the conductivity ?ã as a function of the temperature occurs due to the thermal history of these samples. The saturation magnetic moment (nB) at 5K, of some synthesized CuxNi1-xFe2O4 compounds has been determined. It has been found that nB increases with the nickel content in the ferrite sample.

Preparation of biological samples for transmission electron microscopy is not a trivial task. The samples must withstand a vacuum environment present inside a microscope, and it is often necessary to use non-physiological procedures for their processing. These procedures usually involve aldehyde-based fixation, replacing water with alcohol (i.e. dehydration/substitution), and embedding into a resin, which creates support for the subsequent preparation of thin sections that can be placed into the microscope. In the last decade, the method of cryo-fixation (vitrification) using ultra-fast high-pressure freezing followed by freeze substitution and low-temperature resin embedding gained a dominant position in the cell biology research. In this way, a range of biological samples with a thicknesses up to several hundreds of micrometers was successfully vitrified to a state that was closely related to their in vivo structures. The cryo-fixation of isolated biological objects (with a limited thickness up to several micrometers) is possible in a thin layer of vitrified water by plunge freezing at ambient pressure. In combination with electron cryo-microscopy, this method has become the most effective and fundamental principle for the high-resolution studies and image analysis of fully hydrated samples...

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The Portland Cement Association commissioned a research project at Brigham Young University to compare selected laboratory durability tests available for assessing stabilized aggregate base materials. The laboratory research associated with this project involved two granular base materials, three stabilizers at three concentration levels each, and three durability tests in a full-factorial experimental design. The granular base materials consisted of an aggregate-reclaimed asphalt pavement blend obtained from Interstate 84 (I-84) and a crushed limestone obtained from U.S. Highway 91 (US-91), while the three stabilizer types included Class C fly ash, lime-fly ash, and Type I/II Portland cement. Specimens were tested for durability using the freeze-thaw test, the vacuum saturation test, and the tube suction test. Analyses of the test results indicated that the unconfined compressive strength (UCS) and retained UCS were higher for specimens tested in freeze-thaw cycling than the corresponding values associated with vacuum saturation testing. This observation suggests that the vacuum saturation test is more severe than the freeze-thaw test for materials similar to those evaluated in this research. The analyses also indicated that the I-84 material retained more strength during freeze-thaw cycling and vacuum saturation and exhibited lower final dielectric values during tube suction testing than the US-91 material. Although the I-84 material performed better than the US-91 material, the I-84 material required higher stabilizer concentrations to reach the target 7-day UCS values specified in this research. After freeze-thaw testing, the Class C fly-treated specimens were significantly stronger than both lime-fly ash- and cement-treated specimens. In the vacuum saturation test, none of the three stabilizer types were significantly different from each other with respect to either UCS or retained UCS. Dielectric values measured during tube suction testing were lowest for cement-treated specimens, indicating that cement performed better than other stabilizers in reducing the moisture/frost susceptibility of the treated materials. The results also show that, as the stabilizer concentration level increased from low to high, specimens performed better in nearly all cases. A strong correlation was identified between UCS after the freeze-thaw test and UCS after the vacuum saturation test, while very weak correlations were observed between the final dielectric value after tube suction testing and all other response variables. Differences in variability between test results were determined to be statistically insignificant. Engineers interested in specifying a comparatively severe laboratory durability test should consider vacuum saturation testing for specimens treated with stabilizers similar to those evaluated in this research. The vacuum saturation test is superior to both the freeze-thaw and tube suction tests because of the shorter duration and lack of a need for daily specimen monitoring. Although the Class C fly ash used in this research performed well, further investigation of various sources of Class C fly ash is recommended because of the variability inherent in that material. Similar research should be performed on subgrade soils, which are also routinely stabilized in pavement construction. Research related to long-term field performance of stabilized materials should be conducted to develop appropriate thresholds for laboratory UCS values in conjunction with vacuum saturation testing.