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Thermodynamic and physical properties for high pressure process design
Maša Knez Marevci, 2014, doctoral dissertation

Abstract: The thesis is comprised of three main categories. The first part of dissertation covers investigations of phase equilibria of compounds from natural materials in conventional and also non conventional supercritical fluids. In details, the impact of pressure and/or temperature on the system behaviour (miscibility, solubility, phase inversion) is investigated, quantitative and qualitative analyses to evaluate and identify compounds contained after performing preliminary extraction experiments from different natural tissues are presented. The impact of operating parameters (pre-treatment of the raw material with SFE; different extraction solvents: propane, CO2, non conventional SCFs; different extraction temperatures and pressures) on extraction kinetics is observed. Following substances were taken into consideration: vanillins, caffeine, carnosoic acid extract and lecithin. Second part of dissertation covers studies of phase equilibria of the systems bio oil/gas, which is crucial in biorefinery process design. In this part of dissertation, which covers studies of phase equilibria of binary and ternary systems, the impact of pressure and/or temperature on the system behaviour (miscibility, solubility, phase inversion) for binary system bio oil/supercritical fluid (bio oil/CO2) and (bio oil/H2) was studied. Additionally, phase behaviour of ternary systems of (bio oil/diesel/CO2) and (bio oil/tail water/CO2) under the impact of pressure and/or temperature is observed. These data are of a high importance for bio refineries as an important part of necessary sustainable development. In recent years, studies on biodiesel synthesis have focused on development of process intensification technologies to resolve some of these issues. Fundamental data to design fractionation process of components of bio oil are crucial for an efficient hydrogenation process of bio oil. In the third part of dissertation observation of phase equilibria and determination of the parameters like diffusion coefficient, density and viscosity for the systems polymer/CO2 at elevated pressures is investigated. An overview of different methods applied to determine the parameters like diffusion coefficient, density and viscosity of the systems polymer (PEG)/CO2 at elevated pressures is offered. Observation of phase equilibria of the binary system PEG/CO2, determination of the impact of pressure and/or temperature on the system behaviour (miscibility, solubility, phase inversion), determination of thermodynamically and physically properties of the system with new applicative methods and finally, comparison of the results obtained by different methods is provided. The interfacial tension (IFT) at the (PEG)/CO2 interface has been determined by using an experimental technique developed to study the interfacial interactions of the liquids in equilibrium with gas in a glass-windowed equilibrium cell by the means of Capillary Rise (CR) method. Advantages and disadvantages of methods that were applied are exposed and discussed.
Keywords: phase equilibria, natural materials, conventional and non conventional supercritical fluids, extraction, bio oil, data for biorefinery process design, systems polymer (PEG)/CO2, diffusion coefficient, density, viscosity, surface tension, Capillary Rise (CR) method.
Published in DKUM: 28.10.2014; Views: 2690; Downloads: 362
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Isolation and Characterisation of Flavonoids From Citrus Peels
Katja Makovšek, 2013, doctoral dissertation

Abstract: Citrus flavonoids are very interesting for food and pharmaceutical industry since they possess many antioxidant properties and biological activities. Mandarin peels represent an important source of hesperidin and polymethoxy flavones nobiletin and tangeretin. Pommelo peels represent an important source of naringin that can be used as precursor for naringin dihdydro-2,3-chalcone artificial sweetener. Since pommelo peels possess good antioxidant and antimicrobial properties, their extracts are very interesting products for food industry. Therefore isolation of flavonoid from mandarin and pommelo peels is an important topic of investigations. The investigation of the doctoral dissertation is divided in four parts. The first part is focused on the determination of the optimal conditions for the isolation of hesperidin and naringin from mandarin and pommelo peels by conventional extraction. The optimal conditions and the influence of extraction parameters are determined by Taguchi methodology. Very good isolation efficiency of hesperidin, 61.3 mg HES from 1 g of mandarin peels, was obtained by 70 % acetone solution and extraction conditions: 60 °C, 90 min, material to solvent ratio 1/50 g/mL and 3 stages of extraction. The highest amount of naringin, 32.8 mg NAR were isolated from 1 g of material at conditions: conventional extraction, 120 min, albedo, 60 % ethanol, material to solvent ratio 1/50 g/mL and 60 °C. The simple procedure of conventional extraction shows results comparable to more sophisticated methods such as extraction with microwave and ultrasound. Taguchi experimental design was proved to be an efficient methodology to determine the optimal conditions and the parameters that significantly influence product properties. The second part of the investigation focuses on the characterization of mandarin and pommelo peel extracts and their antioxidant properties. Radical scavenging activity against DPPH and antioxidant capacity of lipid soluble and water soluble compounds were determined for mandarin and pommelo extracts. Taguchi experimental design was applied for determination of the influence of extraction parameters on antioxidant properties. The optimal conditions to prepare extracts with high antioxidant properties were also determined. In the third part the investigation focuses on the concentration and separation of citrus flavonoids by extraction with supercritical fluids. Supercritical CO2 was applied for the separation of polymethoxylated flavones (PMF) and flavanone glycoside from mandarin peels. The optimal conditions and the parameter influence on the separation were determined by using Taguchi experimental design. The influence of supercritical fluid extraction parameters on material pre-treatment and isolation of flavonoids was studied. These investigations show that supercritical CO2 is a potential solvent for isolation and separation of PMF from mandarin peels. The fourth and last part of the investigation focuses on the concentration of flavonoids in extract solutions. Since membrane separation processes are very interesting concentration methods in industry, microfiltration, ultrafiltration, nanofiltration and revese osmosis were used for concentration of mandarin and pommelo peel extract solutions. Microfiltration and ultrafiltration could be used in the separation steps after extraction, since they did not influence the amount of dry material and valuable compounds in tested solutions. Reverse osmosis and nanofiltration were shown as useful methods for separation of solvent from extract solutions.
Keywords: Flavonoids, hesperidin, naringin, citrus peels, mandarin (Citrus reticulata), pommelo (Citrus maxima), conventional extraction, supercritical fluid extraction, membrane separation processes, Taguchi experimental design
Published in DKUM: 22.04.2013; Views: 3692; Downloads: 461
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Isolation and concentration of natural antioxidants with high-pressure extraction
Majda Hadolin Kolar, Andreja Rižner Hraš, Davorin Bauman, Željko Knez, 2004, original scientific article

Abstract: In present work, the purification of crude rosemary extract with supercritical fluids is presented. Carbon dioxide was used as a solvent. The crude extract was prepared from rosemary with conventional extraction process. The supercritical CO2 extraction of crude extracts was performed at pressures 10 and 20 MPa and temperatures 35 and 60 °C. The best results were obtained at pressure 10 MPa and temperature 35 °C. The content of carnosic acid in the samples before and after high pressure extraction was identified by high performance liquid chromatography. The content of carnosic acid in purified extract is higher compared to crude extract. The antioxidative efficiency of extracts was determined by measuring peroxide value. Activity ofpurified rosemary extracts is higher compared to crude extracts.
Keywords: chemical processing, high pressure technology, extraction, CO2, natural antioxidants, rosemary extract, food additives
Published in DKUM: 01.06.2012; Views: 2386; Downloads: 110
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Extraction of phenolic compounds from elder berry and different grape marc varieties using organic solvents and/or supercritical carbon dioxide
Tünde Vatai, Mojca Škerget, Željko Knez, 2009, original scientific article

Abstract: Optimal operating conditions for the extraction of phenolic compounds from grape marc and elder berry have been investigated. The aim was to obtain extracts with high anthocyanin content, which show stability during storage and would be potentially interesting for commercial applications as natural colorants. For this purpose three varieties of grape marc, native to Slovenia (Refošk, Merlot and Cabernet), were studied. The results were compared with the extraction of elder berry, which is known for its high anthocyanin content. Single-step batch extractions were performed with ethanol, ethyl-acetate and acetone in different ratios with water. Temperatures of 20 °C, 40 °C and 60 °C were applied. Influence of the change in pH values of the extraction media was investigated regarding the yield and degradation of anthocyanins. Two-step extractions, combining supercritical fluid extractions (SFE) and conventional batch extractions, were applied. The most efficient conventional solvents in single-step extractions were mixtures of organic solvent and water at 60 °C. Pre-treatment of the natural material with supercritical CO2 (with or without ethanol as co-solvent) improved the extraction of polyphenols from the grape marc. This method provides an alternative to the pre-treatment of the plant materials, replacing toxic organic solvents (e.g. hexane). Acidified extraction media resulted in higher anthocyanin content in the extracts. However, the degradation of the anthocyanins during storage was higher, which led to the loss of the intensive colour. The addition of a commercially available rosemary extract to the extraction solvent improved the stability of the grape marc extract during storage.
Keywords: extraction, organic solvents, supercritical CO2, anthocyanins, grape marc, elder berry, natural colorant
Published in DKUM: 01.06.2012; Views: 1883; Downloads: 121
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Separation of parthenolide from feverfew: performance of conventional and high-pressure extraction techniques
Lucija Čretnik, Mojca Škerget, Željko Knez, 2005, original scientific article

Abstract: In present work the extraction of feverfew flower heads was performed using supercritical carbon dioxide at pressures from 200 to 800 bar and at temperatures of 40, 60 and 80 °C. For comparison, the conventional extractionswith organic solvents have been performed. Dry feverfew flower heads were used as starting material. Supercritical fluid extraction (SFE) wasperformed using a semi continuous flow apparatus in a laboratory and pilot scale. The influence of process parameters on the total yield and amount of parthenolide isolated was investigated. Dynamic behaviour of the extraction runs followed by single-step separation was analysed by a mathematical model for initial constant rate extraction period and the subsequent time-dependant diffusion controlling mass transfer rate period. In order to concentrate the obtained extract in parthenolide, a two-step separation was employed.
Keywords: chemical processing, high pressure extraction, conventional extraction, supercritical CO2, parthenolide, feverfew, extraction rate, mass transfer
Published in DKUM: 01.06.2012; Views: 1920; Downloads: 106
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Phenols, proanthocyanidins, flavones and flavonols in some plant materials and their antioxidant activities
Mojca Škerget, Petra Kotnik, Majda Hadolin Kolar, Andreja Rižner Hraš, Marjana Simonič, Željko Knez, 2005, original scientific article

Abstract: Methanol extracts prepared from five plant materials native to the Mediterranean area, namely olive tree (Olea europaea) leaf, St. John's wort (Hypericum perforatum), hawthorn (Crataegus laevigata), oregano (Origanum vulgare) and laurel leaf (Lauris nobilis), were examined for their phenolic components. Total phenolic content was determined by the Folin-Ciocalteu method. The content of proanthocyanidins in acid-hydrolysed extracts was determined spectrophotometrically. The contents of free flavones (apigenin andluteolin) and flavonols (kaempferol, myricetin and quercetin) were determined by HPLC analysis. The time of hydrolysis of flavones, flavonols andproanthocyanidins was optimised. Antioxidant activities of apigenin, luteolin, kaempferol, myricetin, quercetin and of plant extracts were examined. Antioxidative activities were studied in sunflower oil at 98 °C, by measuring peroxide value, and in an aqueous emulsion system of -carotene and linoleic acid by measuring the absorbance of the sample. Among flavones and flavonols investigated, only myricetin inhibited oxidation of sunflower oil. All other flavones and flavonols showed pro-oxidative activity. Oppositely, in the emulsion system, only apigenin showed pro-oxidative activity while otherflavones and flavonols and plant extracts inhibited oxidation of -carotene.
Keywords: chemical processing, extraction, plant material, fenolic content, hidrolysis, antioxidants, flavones, flavonols, proanthocyanidines, oils, emulsions
Published in DKUM: 01.06.2012; Views: 2453; Downloads: 122
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Chemical composition of Juniperus communis L. fruits supercritical CO2 extracts: dependence on pressure and extraction time
Branislava Barjaktarović, Milan Sovilj, Željko Knez, 2005, original scientific article

Abstract: Ground fruits of the common juniper (Juniperus communis L), with a particle size range from 0.2500.400 mm, forming a bed of around 20.00 +/- 0.05 g, were extracted with supercritical CO2 at pressures of 80,90, and 100 bars and at a temperature of 40 De. The total amount of extractable substances or global yield (mass of extract/mass of raw material) for the supercritical fluid extraction process varled from 0.65 to 4.00"10 (wt). At each Investigated pressure, supercriticaI CO2 extract fractions collected In successive time intervals over the course of the extraction were analyzed by capillary gas chromatography, using flame ionization (GO-FIO) and mass spectrometric detection (GC-MS). More than 200 constituents were detected In the extracts, and the contents of 50 compounds were reported in the work. Dependence of the percentage yields of monoterpene, sesquiterpene, oxygenated monoterpene, and oxygenated sesquiterpene hydrocarbon groups on the extraction time was investigated, and conditions that favored the yielding of each terpene groups were emphasized. At all pressures, monoterpene hydrocarbons were almost completely extracted from the berries in the first 0.6 h. It was possible to extract oxygenated monoterpenes at 100 bar in 0.5 h and at 90 bar in 1.2 h. Contrary to that, during an extraction period of 4 h at 80 bar, it was possible to extract only 75% of the maximum yielded value of oxygenated monoterpene at 100 bar. Intensive extraction of sesquiterpenes could be by no means avoided at any pressure, but at the beginning of the process (the first 0.5 h) at 80 bar, they were extracted about a and 3 times slower than at 100 and 90 bar, respectively. Oxygenated sesquiterpenes were yielded at fast, constant extraction rates at 100 and 90 bar In 1.2 and 3 h, respectively. This initial fast extraction period was consequently foIlowed by much slower extraction of oxygenated sesquiterpenes.
Keywords: chemical processing, high pressure technology, CO2, supercritical fluid extraction, pressure, extraction time, Juniperus communis, oxygenated terpenes, juniper berry oil, carbon dioxide
Published in DKUM: 01.06.2012; Views: 2020; Downloads: 54
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Optical properties of plastically deformed copper
J. Trajić, Rebeka Rudolf, Ivan Anžel, M. Romčević, N. Lazarević, M. Mirić, Z. Lazarević, B. Hadžić, Nebojša Romčević, 2010, published scientific conference contribution

Abstract: Pure copper (99.99), prepared in the sample of square cross-section (10 x 10 mm2) and length about 50 mm, was extremely plastically deformed with the repeated application of Equal Channel Angular Pressing (ECAP). ECAP was applied as an effective technique for producing bulk nano-scaled structures. Optical properties of the sample were investigated using Raman spectroscopy. Two types of lines: narrow (with width of 7 cm¡1) and wide ( 40 cm¡1) are registered. Existence of two types of lines indicates that in the specimen exists nano-sized crystal structures of both Cu and CuO related with three dimensional amorphous boundary spaces, which indicates that plastic deformation of the sample did not lead to total amorphisation of the specimen.
Keywords: plastically deformed copper, hydrometallurgical extraction of metals
Published in DKUM: 31.05.2012; Views: 2061; Downloads: 116
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Ellipsometric measurements of plastically deformed copper
M. Mirić, Rebeka Rudolf, Ivan Anžel, B. Hadžić, M. Romčević, J. Trajić, Nebojša Romčević, 2009, published scientific conference contribution

Abstract: Chemically pure copper (99.99) prepared in the sample of square cross-section (10 x 10 mm2) and length about 50 mm was extremely plastically deformed with the repeated application of equal channel angular pressing. Equal channel angular pressing was applied as an effective technique for producing bulk nanoscaled structures. It is well known that severe plastic deformation of metallic materials often leads to microstructure with ultrafine grains and cross-sections which remain about equal before and after deformation. Optical properties of the sample were studied using spectroscopic ellipsometry in UV-VIS range. The parameters of the sample like copper oxide and surface roughness overlayer were calculated using two-film model together with the Bruggeman effective medium approximation.
Keywords: hydrometallurgical extraction of metals, copper
Published in DKUM: 31.05.2012; Views: 1743; Downloads: 141
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