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.

The Portland Cement Association commissioned a research project at Brigham Young University to compare selected laboratory durability tests available for assessing stabilized subgrade materials. Improved understanding of these tests is needed to enable more objective selection of durability tests by design engineers and to facilitate more meaningful comparisons of data obtained for different stabilizer treatments using different evaluation procedures. The laboratory research associated with this project involved two subgrade materials, four stabilizers at three concentrations each, and three durability tests in a full-factorial experimental design. The two subgrade soils used were a silty sand and a lean clay, while the four stabilizer types included Class C fly ash, lime-fly ash, lime, and Type I/II portland cement. The three tests used in this comparative study were the freeze-thaw test, the vacuum saturation test, and the tube suction test. On average, to achieve the same 7-day unconfined compressive strength (UCS) values, the sand required 4.4 times more Class C fly ash than cement, 3.6 times more lime-fly ash than cement, and 6.0 times more lime than cement. Likewise, the clay required 10 times more Class C fly ash than cement, 7.5 times more lime-fly ash than cement, and 1.8 times more lime than cement. Analyses of the test results indicated that the UCS and retained UCS were higher for specimens tested by vacuum saturation than the corresponding values associated with freeze-thaw cycling. This observation suggests that the freeze-thaw test is more severe than the vacuum saturation test for these particular fine-grained materials. Testing also suggested that specimens with 7-day UCS values below 200 psi will generally not survive freeze-thaw cycling. After both freeze-thaw and vacuum saturation testing, the sand specimens treated with lime-fly ash had significantly higher UCS and retained UCS than specimens treated with Class C fly ash, lime, or cement. Similarly, the clay specimens treated with Class C fly ash or lime-fly ash had significantly higher UCS values than specimens treated with cement or lime; however, clay specimens treated with Class C fly ash and lime-fly ash were not significantly different. None of the four stabilizer types were significantly different from each other with respect to retained UCS after vacuum saturation testing. Dielectric values measured in tube suction testing were lowest for specimens treated with lime-fly ash and cement with respect to the sand and for specimens treated with Class C fly ash and cement with respect to the clay. The lime-fly ash and cement successfully reduced the dielectric value of sand specimens to a "marginal" rating, while no stabilizer reduced the moisture susceptibility of the clay to a satisfactory level. 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 in an analysis of the CVs associated with data collected in this research. Although the freeze-thaw test utilized in this research was determined to be more severe than the vacuum saturation test for materials similar to those tested in this study, the vacuum saturation test is recommended over both the freeze-thaw and tube suction tests because of the shorter test duration, usability for specimens with 7-day UCS values even below 200 psi, and lack of a need for daily specimen monitoring.