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Dušica Mirković, 2019, doktorska disertacija

Opis: The aim of this doctoral research was to develop and optimize parenteral nanoemulsions as well as the total parenteral nutrition (TPN) admixture containing a nanoemulsion obtained in the course of the optimization process (hereinafter referred to as optimal nanoemulsion), and to examine their physicochemical and biological quality as well. In addition, the quality of the prepared nanoemulsions was compared with the quality of the industrial nanoemulsion (Lipofundin® MCT/LCT 20%), and, in the end, the TPN admixture initially prepared was also compared with the admixture into which the industrial emulsion was incorporated. Parenteral nanoemulsions that were considered in this dissertation were prepared by the high-pressure homogenization method. This method is the most widely applied method for the production of nanoemulsions due to the shortest length of homogenization time, the best-obtained homogeneity of the product and the smallest droplet diameter. For the nanoemulsion formulation, preparation and optimization purposes, by using, firstly, the concept of the computer-generated fractional design, and, after that, the full experimental design, the assessment of both direct effects of different formulation and process parameters (the oil phase type, the emulsifier type and concentration, a number of homogenization cycles and the pressure under which homogenization was carried out) as well as the effects of their interactions on the characteristics of prepared nanoemulsions was performed. Monitoring the nanoemulsion physical and chemical stability parameters was carried out immediately after their preparation, and then after 10, 30 and 60 days. It included the visual inspection, the measurement of the droplet diameter (the mean and volume droplet diameter), the polydispersity index, the ζ-potential, the pH value, the electrical conductivity, and the peroxide number. After the preparation and after 60 days, the biological evaluation (the sterility test and the endotoxic test) of the prepared nanoemulsions was carried out. As far as the characterization of the TPN admixture is concerned, it included practically the same parameters. The dynamics of monitoring the characteristics of the TPN admixture was determined on the basis of practical needs of hospitalized patients (0h, 24h and 72h). The scope and comprehensiveness of this issue indicated the need to divide the doctoral dissertation into three basic stages. The first stage was preliminary. Using the 24-1 fractional factorial design, nanoemulsions for the parenteral nutrition were prepared. They contained either a combination of soybean and fish oil, or a combination of medium chain triglycerides and fish oil. In addition, the type and the amount of an emulsifier used, a number of high-pressure homogenization cycles, and the homogenization pressure, were also varied. The measurement of the above-mentioned parameters for the industrial nanoemulsion was parallely carried out (Lipofundin® MCT/LCT 20%). The objective of this part of the research was to identify critical numerical factors having the most significant effect on the characteristics that define the prepared parenteral nanoemulsions. Parameters that were singled out as the result of this stage of the research (the emulsifier concentration and a number of homogenization cycles) were used as independent variables in the second stage of the research.
Ključne besede: nanoemulsions, total parenteral nutrition admixtures, high pressure homogenization, design of experiments, optimization, analysis of variance, artificial neural networks
Objavljeno: 07.06.2019; Ogledov: 10810; Prenosov: 0
.pdf Celotno besedilo (2,82 MB)

A new method for testing the anti-permeability strength of clay failure under a high water pressure
Fu-wei Jiang, Ming-tang Lei, Xiao-zhen Jiang, 2015, izvirni znanstveni članek

Opis: It is difficult to judge the failure of clay seepage under a high water pressure.This paper presents a new method to assess clay failure based on the anti-permeability strength, which is the critical water pressure to destroy the clay. An experiment is designed to test the value that avoids the problem of the time-consuming, traditional method to test clay seepage deformation. The experimental system and the process of testing are introduced in this paper. With a self-designed experimental system and method, 18 groups of sample were tested. The results show that the clay thickness and the seepage paths influence the anti-permeability strength. It also indicates that water infiltrates into the clay under the condition that its pressure exceeds a minimum value (P0).
Ključne besede: clay failure, seepage deformation, anti-permeability strength, high water pressure
Objavljeno: 15.06.2018; Ogledov: 538; Prenosov: 29
.pdf Celotno besedilo (249,24 KB)
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Yielding in the isotropic compression of Porto silty sand
Miguel Ferreira Amaral, Sara Rios, António Viana da Fonseca, 2012, izvirni znanstveni članek

Opis: The yielding locus of a well-graded silty sand was analysed by means of isotropic compression tests and scanning electron microscopy (SEM). The tests were performed with precise instrumentation, for internal and external strain measurements, and shear-wave velocity measurements by means of bender elements. Finally, aiming at an accurate evaluation of the yield stress, four different methods were applied – two quite well know and the other two being innovative – leading to interesting conclusions.
Ključne besede: silty sand, yield point, isotropic compression, high pressure, seismic waves
Objavljeno: 13.06.2018; Ogledov: 344; Prenosov: 53
.pdf Celotno besedilo (613,18 KB)
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Determining the speed of sound, density and bulk modulus of rapeseed oil, biodiesel and diesel fuel
Boban Nikolić, Breda Kegl, Saša Marković, Melanija Mitrović, 2012, izvirni znanstveni članek

Opis: Modern tendencies in the development of diesel engines include the operation of the system for injecting diesel fuel at pressures higher than 100 MPa. Knowing the characteristics of liquid fuels such as speed of sound, bulk modulus and density depending on pressure, is important for predicting the behavior of fuel injection systems for diesel engines and optimization of the same. The paper presents an original method and apparatus (device) for determining the speed of sound and density of fluids depending on the pressures. With this method, values of these characteristics for rapeseed oil, biodiesel and conventional diesel fuel at pressures up to 160 MPa are determined. The method is non-destructive, it can also be applied to higher pressures than 160 MPa, as well as other liquid fluids that are used at high pressure - hydraulic oil, for example.
Ključne besede: biodiesel, rapeseed oil, speed of sound, bulk modulus, density, high pressure
Objavljeno: 07.07.2017; Ogledov: 591; Prenosov: 278
.pdf Celotno besedilo (405,37 KB)
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Process design for flavour encapsulation into carbohydrate melts using high pressure homogenizer
Urban Feguš, 2016, doktorska disertacija

Opis: The aim of the research project was to develop encapsulated flavourings suitable for the final food applications such as chewing gums, instant teas and confectionary products. For this purpose that water soluble particles with particle size distribution 400-1500 µm and flavour loading up to 30 wt. % should be developed. In order to produce encapsulates with desired physical properties research work was divided into three project phases. The scope of Phase 1 was to select suitable carrier materials and to perform preliminary experiments using laboratory scale process set-up. Different carbohydrates (maltodextrin, simple sugars and sugar syrups) were tested and selected according to their physical characteristics and their process performance. Afterwards preliminary experiments were performed by using laboratory scale set-up. Observations were used for defining process parameters for the design and construction of the pilot plant. Phase 2 covered design and development of the pilot plant for flavour encapsulation while In Phase 3 different process parameters were tested. In the first part influence of the process parameters (processing temperature, homogenizing pressure, mass flow, temperature of the cooling media, retention time in the cooling media and ratio between cooling media and product) on the encapsulation efficiency was investigated. Experiments were performed according to the Design of Experiments (DoE) analysed using analysis of covariance (ANCOVA). Process temperature, pressure at second homogenization step and residence time in cooling media had significant effect on the encapsulation efficiency while pressure at first homogenizing step, mass flow, temperature of the cooling media and ratio between product and cooling media were nonsignificant. Increase in the process temperature (T>130 °C) resulted in paste-like product with increased moisture content up to 13,3 wt.% which was not suitable for further processing. On the other hand samples processed at lower temperature (T<130 °C) resulted in crystalline-like structure with low moisture content. Low flavour retention (<4,5 %) was observed within all samples. Results obtained by ANCOVA were used for further optimization of the process parameters (e.g. homogenizing pressure and the retention time in the cooling media). Maximum flavour load of 3,5 % was observed regardless the homogenizing pressure. Low encapsulation efficiency (η<35 %) was related to poor emulsion stability. Additionally, effect of expansion pressure on the particle size distribution was investigated. It was observed that particle size distribution was little affected by varying expansion pressure (nozzle diameter). All formulation showed similar particle size distribution in-between 40-440 µm. In the last section effect of the emulsifier, flavouring properties and carrier were studied. Emulsifiers with different HLB values were tested in order to increase encapsulation efficiency. Flavourings were selected on the basis of their composition (polarity and volatility). For the encapsulation experiments mentha arvensis oil, orange oil and compounded pineapple flavouring were used. As an alternative carrier material erythritol was used. Addition of emulsifier improved flavour retention for samples containing mentha arvensis oil, while no affect was observed within samples containing orange oil and pineapple flavouring due to the volatility and diffusion of active compounds from matrix to surrounding environment.
Ključne besede: encapsulation, carbohydrate melts, flavouring, high pressure homogenizer
Objavljeno: 25.07.2016; Ogledov: 1442; Prenosov: 94
.pdf Celotno besedilo (4,56 MB)

Volumetric properties of ethanol-water mixtures under high pressure
Aljana Petek, Darja Pečar, Valter Doleček, 2001, izvirni znanstveni članek

Opis: Densities of ethanol-water mixtures have been measured using a vibrating tube densimeter and a different arrangement high-pressure experimental set-up. Measurements were carried out at 298,15 K in a pressure range from 0.1 MPa to 5MPa. Partial molar volumes, excess molar volumes and coefficients of isothermal compressibility were calculated. The molar volumes of alcohol and its partial molar volumes in mixtures with water are found to decrease monotonously with increasing pressure. Excess molar volumes are negative at all pressures. The numerical P-V relations at each composition are correlated satisfactorily as a function of pressure by the Hayward equation.
Ključne besede: chemistry, high-pressure vibrating tube densimeter, excess molar values, isothermal compressibility
Objavljeno: 10.07.2015; Ogledov: 748; Prenosov: 50
.pdf Celotno besedilo (424,02 KB)
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Pressure stability of lipases and their use in different systems
Maja Leitgeb, Željko Knez, 2001, izvirni znanstveni članek

Opis: For the investigation of the solvent impact on the enzymes, lipases from different sources (Pseudomonas fluorescences, Rhizopus javanicus, Rhizopus niveus, Candida rugose and Porcine pancreas) were used. Stability and activity of these lipases in aqueous medium in supercritical $CO_2$ and liquid propane at 100 bar and 40°C were studied. On the basis of previous results lipases were used for their application in two different systems. The application of the polysulphone membrane in the continuous stirred tank membrane reactor was studied on the model system of the hydrolysis of oleyl oleate in propane at high pressure. As a catalyst the Candida rugosa lipase was used. The next utilization of lipases was the use of on silica arerogel self-immobilized lipase from Porcine pancreas as catalyst for esterification reaction in near-critical propane at 40°C and 100 bar.
Ključne besede: chemical processing, supercritical fluids, lipases, enzyme stability, high pressure membrane reactor
Objavljeno: 10.07.2015; Ogledov: 823; Prenosov: 113
.pdf Celotno besedilo (608,04 KB)
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Particles formation and particle design using supercritical fluids
Željko Knez, Eckhard Weidner, 2003, pregledni znanstveni članek

Opis: Major recent advances. Particle formation and design of solid particles and powdery composites with unique properties is at the moment a major developmentof supercritical fluids (synonymsČ dense gasses, dense fluids, highpressure) applications. This review will focus on recent advances and on fundamentals of these processes and their applications.
Ključne besede: chemical processing, high pressure technology, micronization, supercritical fluids, micro-particles, nano-particles, powder generation, crystallization, particles from gas saturated solutions
Objavljeno: 01.06.2012; Ogledov: 2736; Prenosov: 85
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Multifunctional composites by high-pressure spray processes
Eckhard Weidner, Marcus Petermann, Željko Knez, 2003, pregledni znanstveni članek

Opis: A series of spraying processes designed to generate powders and composites using supercritical fluids have been proposed in the past 15 years. In this review, thermo- and fluid-dynamic aspects and engineering principles are discussed and advantages of such technologies are demonstrated. These new techniques display convincing advantages, producing competitive high-quality products with tailor-made properties. Initial industrial applications have been achieved in the production of food products and fine-chemicals.
Ključne besede: chemical processing, high pressure technology, micronization, supercritical fluids, particles, powder generation, thermodynamics, fluid dynamics, PGSS
Objavljeno: 01.06.2012; Ogledov: 1776; Prenosov: 79
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Preparation of WO[sub]3 aerogel catalysts using supercritical CO[sub]2
Zoran Novak, Petra Kotnik, Željko Knez, 2004, izvirni znanstveni članek

Opis: Single tungsten oxide aerogels (WO3), binary oxide aerogels (WO3-Al2O3) and ternary oxide aerogels (WO3-SiO2-Al2O3) were prepared using standard sol-gel route. Tungsten oxide tetraethoxide (WO(OCH2CH3)4) was used as the sol-gel precursor. The excellent properties of the gels obtained by the sol-gel synthesis were preserved upon supercritical drying with CO2. After supercritical drying at 40 °C and 100 bar, all aerogels were calcined to 800 °C. The influence of the synthesis parameters on the catalytic activity of WO3as supported on silica andžor alumina aerogels was investigated through thetransformation of N-(phosphonomethyl)iminodiacetic acid to N-(phosphonomethyl)glycine. Despite including WO3 into single and mixed silicaand alumina aerogels, high specific surface areas (284-653 m2 g-1) were preserved. Higher conversion was obtained for catalysts with higher ratios of WO3 in the mixed silica-alumina aerogels that were calcined at 800 °C.
Ključne besede: chemical processing, aerogels, catalysts, tungsten oxides, preparation of aerogels, characterisation of aerogels, supercritical CO2, supercritical drying, high pressure technology
Objavljeno: 01.06.2012; Ogledov: 1366; Prenosov: 27
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