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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
1

Process intensification : spinning disc reactor for the polymerisation of styrene

Boodhoo, Kamelia January 1999 (has links)
This investigation is concerned with the assessment of the performance of a novel spinning disc reactor (SDR) for the polymerisation of chemically initiated freeradical polymerisation of styrene. The application of high acceleration fields such as those created on the surface of the grooved rotating disc to the polymerising system is aimed at intensifying the polymerisation rate and producing a better quality polymer product. As part of the experimental programme, four separate sets of experimental runs were conducted on a 360 mm diameter grooved rotating disc at a fixed temperature of 88-90°C to explore the effects of disc rotational speed and prepolymer feed conversion/viscosity on the extent of monomer conversion and molecular weight properties (M., MW and MWD) of the product from the SDR. The performance data of the SDR was compared with conventional batch polymerisation data. Both the disc rotational speed and prepolymer feed conversion/viscosity variables were found to have a profound influence on the performance of the SDR. A steady increase in conversion, rate of polymerisation and hence time saving in one pass in the SDR were observed with a rise in the prepolymer feed conversion and rotational speed until, for the latter, an optimal speed of rotation which gave the highest rate of polymerisation was reached. The results have been explained in relation to the effect of disc speed and prepolymer feed viscosity on mean film thickness, mean residence time and film surface instabilities. Furthermore, the SDR product is seen to have generally improved characteristics in terms of narrower molecular weight distribution when compared to polymer prepared in the batch at the same conversion. The large enhancement of the rate of styrene polymerisation in the SDR was discussed in terms of a possible improvement in the BPO initiator efficiency f and non-stationary state polymerisation conditions likely to be prevalent on the rotating disc. The general improvement in SDR product quality was ascribed to the combined effects of a reduced diffusion path length and an intense mixing mechanism within the thin film. A separate experimental study exploring the effects of micromixing efficiency on the conversion and molecular weight properties of styrene polymerisation in the batch was also undertaken. The opposing effects of enhanced micromixing in batch and continuous polymerisation systems were contrasted in a theoretical manner. A theoretical case study highlighting the energy efficiency of the SDR was also carried out. Savings in energy of more than 70% was calculated for a semi-batch process using an industrially adapted spinning disc reactor in comparison to a purely batch process. Finally, a two-stage continuous industrial process for free-radical polymerisation has been proposed consisting of an enhanced tubular reactor in the first stage followed by a parallel arrangement of several rotating disc surfaces. Improvements in intrinsic safety and minimised risks of polymer degradation and thermal runaways are the expected potential benefits. Keywords: Process Intensification, Thin Film, Spinning Disc Reactor, Free Radical Polymerisation, Polystyrene
2

Volatility and number measurement of diesel engine exhaust particles

Bernemyr, Hanna January 2007 (has links)
Today, emission legislations for engine exhaust particles are mass based. The engines of today are low-emitting with respect to particle mass, with the emissions approaching the detection limit of the current measurement method. This calls for new and improved measurement methods. Both from the point of view of the engine developers and regarding human health effects, particle number seem to be the particle property of greatest interest to legislate upon. Recently, a proposal for a new particle number based measurement methodology has been put forward by the United Nations Economic Commission for Europe (UN ECE). The gas and particle mixture (the aerosol) of engine exhaust is not a stable system. The size and the number of the particles change over time as the temperature and pressure change. Particle number measurements call for dilution which changes the gas-phase concentrations of the condensing gases. The dilution process alters the conditions in the aerosol and thereby influences the measurements. Within the current project it was desired to better understand the outcome of particle number measurements and the complexities of particle sampling, dilution and conditioning prior to measurements. Two experimental set-ups have been developed within the project. The first system includes a rotating disc diluter followed by a volatility Tandem Differential Mobility Analyser (v-TDMA). The second set-up, called the EMIR-system, includes ejector diluters in series followed by a stand-alone Condensation Particle Counter (CPC). After the development of these experimental set-ups, the v-TDMA has been used to study the volatility and the size distributed number concentration of exhaust particles. The EMIR-system was used for total number concentration measurements including only the solid fraction of the aerosol. The experimental work has given practical experience that can be used to estimate the benefits and disadvantages of upcoming measuring methodology. For the engine developers, in order to produce engines that meet future legislation limits, it is essential to know how the measurement procedure influences the aerosol. In summary, the experimental studies have shown that the number of nucleation mode particles is strongly affected by varied dilution. No upper threshold value of the dilution has been found where the dilution effect diminishes. The volatility studies have shown that it is mainly the nucleation mode particles that are affected by heat. The v-TDMA instrument have shown to be a sensitive analytical tool which, if desired to use for further engine exhaust particle characterization, needs some development work. Experimental work with the EMIR-system, which in principle is similar to the instruments proposed for a future standard, shows that these types of measurement systems are sensitive to small changes in the detector cut-off. The major outcome of the project lies in the new detailed knowledge about particle number measurements from engines. / QC 20100628
3

Projeto, fabricação e operação de uma máquina de ensaio de erosão por cavitação

Miranda, Charles Zanini 18 December 2007 (has links)
Made available in DSpace on 2016-12-08T17:19:32Z (GMT). No. of bitstreams: 1 Parte 1_CAPA.pdf: 112741 bytes, checksum: 77f664f41fd325d0dc88d0a1e1c7d4fe (MD5) Previous issue date: 2007-12-18 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The present work deals with the design, fabrication and operation of a cavitation erosion equipment and with the preliminary results obtained by its testing. A new cavitation erosion testing machine was designed, fabricated and tested, using a rotating disc with holes for generating cavitation. The developed equipment has as main advantages, in relation to the existing ones, low fabrication cost due to its smaller size and reduced number of components, the specimen quantity of up eight per test and a lower power needed to carry out the testing. It is small size equipment, capable of generating the necessary bubbles for causing the erosion by cavitation on the specimen surfaces at the speed of 4400 rpm and maximum power of 30 kW. Two types of rotating discs were investigated: with cavitation inducers holes and with pins. The rotating disc with inducer holes was more efficient as its power consumption was only 14 kW and the disc with inducer pins was 23 kW for practically the same erosion rate obtained by bronze and aluminium, both at the rotation speed of 4400 rpm. The cavitation erosion is responsible for surface damage caused exposure to this phenomenon. The equipment is capable of testing simultaneously 8 specimens of different materials, what shows the variety of possible materials which can be performed simultaneously in short period of time. The specimen erosion was confirmed by its loss of mass, using an analytical balance with accuracy of 0,2 mg and by the analyses of the eroded surface through the photograph analyses from the scanning electron microscope, MEV. The occurrence of cavitation due to micro-jets impact was confirmed by the microphotographs of circular craters in the aluminium specimens. The tested and discussed materials in this work presented different behavior when exposed to cavitation erosion. Bronze and brass showed a practically constant and linear erosion rate as seen in the lost mass versus testing time graphs. But, aluminium presented much lower wear, except for 10 to 15 hours of testing. After this period of time, a substantial reduction in the wear rate was occurred due to the formation of a fine layer of alumina which provided an increase in the aluminium wear resistance. According to the results obtained by the nodular cast iron specimens, it was observed that the cemented layer increased the erosion resistance to cavitation and decreased the specimen surface oxidation, however, the occurrence of surface oxidation prejudiced a more accurate analyses. / O presente trabalho consiste no projeto, construção e operação de uma máquina de ensaio de erosão por cavitação e dos primeiros resultados obtidos por meio deste equipamento. Um novo conceito de máquina de ensaio de erosão por cavitação foi projetado, construído e ensaiado, usando um disco rotativo com furos e pinos indutores de cavitação. O equipamento projetado possui como principais vantagens, em relação aos equipamentos já existentes, o baixo custo de fabricação devido ao menor tamanho do equipamento, número reduzido de componentes, a quantidade de até oito amostras por ensaio e a menor potência necessária para realização dos ensaios. Trata-se de uma máquina de pequeno porte, capaz de gerar as bolhas necessárias para o surgimento da erosão por cavitação nas superfícies dos corpos de prova na rotação de até 4400 rpm e potência máxima de 30 kW. Foram investigados dois tipos de discos rotativos: com furos indutores e com pinos indutores de cavitação. O disco rotativo com furos indutores foi mais eficiente, pois consumiu a potência de 14 kW e com pinos indutores a potência consumida foi de 23 kW, para a mesma rotação de 4400 rpm, e apresentaram praticamente a mesma taxa de erosão verificada no bronze e alumínio. A erosão por cavitação é responsável por danos causados nas superfícies expostas a este fenômeno. O equipamento é capaz de ensaiar simultaneamente 8 corpos de prova de diferentes materiais, o que demonstra a variedade possível de materiais de estudos que podem ser feito em conjunto, em reduzidos períodos de tempo. A erosão nos corpos de prova foi verificada pela perda de massa, usando uma balança analítica de precisão 0,2 mg, e pela análise da superfície erodida através da análise das fotografias obtidas no microscópio eletrônico de varredura, MEV. A ocorrência da cavitação por impacto de micro-jatos foi comprovada com as micro-fotografias de crateras circulares nas amostras de alumínio. Os materiais ensaiados e discutidos neste trabalho apresentaram comportamentos diferentes quando exposto à erosão por cavitação. O bronze e o latão tiveram uma taxa de erosão praticamente constante e linear demonstrada nos gráficos de perda de massa em relação ao tempo de ensaio. Já o alumínio apresentou um desgaste muito inferior, mas acentuado entre 10 e 15 horas de ensaio. Após este período ocorreu. uma redução significativa na taxa de desgaste, devido a formação de uma fina camada superficial de alumina que conferiu um aumento na resistência ao desgaste do alumínio. De acordo com os resultados obtidos com os corpos de prova em ferro fundido nodular, constata-se que a camada de cementação aumentou a resistência à erosão por cavitação e visivelmente diminuiu a oxidação superficial dos corpos de prova, porém a oxidação superficial ocorrida nestas amostras comprometeram uma análise mais apurada.
4

Start-up and shock loading characteristics of a rotating biological contactor package plant

Fry, Farley Farrel January 1982 (has links)
A full-scale rotating biological contactor treatment system primarily used for treatment of wastes from single-family dwellings was studied at the Blacksburg-Virginia Tech wastewater treatment plant. Municipal primary clarifier effluent was pumped into the 600 gpd rated RBC unit at the rate of 480 gpd for a period of 4 1/2 months. The RBC unit contained a primary clarifier, four stages of discs, and a secondary clarifier. A thorough sampling and analysis program was performed to determine start-up characteristics and resistance to controlled shock loadings. Samples from seven locations, ranging from the influent through each stage of the RBC into the effluent, were collected and analyzed in order to monitor treatment performance. Samples were analyzed for COD, TKN, NH₃-N, Org-N, NO⁻₃-N, SS, DO and total alkalinity. Based on an analysis of the results obtained it was determined that a start-up period of approximately 30 days was required to develop a sufficient growth of biofilm mass to reach"steady state" conditions, i.e., maximum consistent organic removal and nitrification efficiency. Shock loading investigations included step increases in hydraulic and organic loads as well as controlled diurnal flow patterns. From these studies it was determined that the RBC was resistant to changes in effluent organic concentration, but that nitrification efficiency could be notably suppressed. The attached biofilm was not adversely affected by the shock loads. Throughout the manuscript diagrams and tables are provided to clarify procedures and materials used. Analytical results are presented in three-dimensional plots to illustrate patterns revealed by the data. / Master of Science
5

Balanços populacionais de gotas e transferência de massa em colunas de discos rotativos aplicados à desacidificação de óleos vegetais / Drop population balances and transfer in rotating disc columns applied to vegetable oils deacidification

Sanaiotti, Guilherme, 1983- 16 August 2018 (has links)
Orientador: Eduardo Augusto Caldas Batista / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-16T00:41:25Z (GMT). No. of bitstreams: 1 Sanaiotti_Guilherme_M.pdf: 2559183 bytes, checksum: 49e8656b4f14ee53f65b1a0dc45c232d (MD5) Previous issue date: 2010 / Resumo: A desacidificação de óleos vegetais por extração líquido-líquido apresenta-se como uma alternativa atraente às elevadas perdas e gastos energéticos usualmente encontrados nos métodos de refino alcalino e por destilação de ácidos graxos livres, respectivamente. A utilização de insumos provenientes de fontes renováveis e a ausência de geração de resíduos conferem ainda caráter ambiental pertinente ao processo. Modelos descritivos de perfis axiais de composição de fases, fundamentados em balanços populacionais de gotas e transferência de massa multicomponente, são essenciais para o desenvolvimento de métodos de design e scale up de colunas de extração líquido-líquido. A principal finalidade deste trabalho foi avaliar correlações, métodos e diretrizes para o dimensionamento de colunas de discos rotativos aplicadas à desacidificação de óleo de soja. Dados de composições de fases em equilíbrio, densidades, viscosidades e tensões interfaciais de sistemas compostos por óleo de soja + ácido linoléico comercial + etanol + água a 298,2 K foram determinados experimentalmente a frações mássicas de água no solvente iguais a 5,00 %, 8,00 %, 11,00 % e 14,00 %. Os desvios relativos absolutos entre os valores experimentais e os estimados por meio de equações empíricas foram inferiores a 6,36 %. Perfis de composição de fases quantificados por 3 diferentes modelos foram correlacionados a dados experimentais existentes na literatura, determinados em uma coluna de discos rotativos (RDC) com 5,0 cm de diâmetro, utilizada para a desacidificação de óleo de milho. Os desvios relativos absolutos entre as frações mássicas de ácidos graxos livres experimentais e as obtidas por simulação foram próximos a 20 %. Em um estudo hipotético, colunas de discos rotativos foram dimensionadas sob diferentes condições operacionais e teores de água no solvente, ao se considerar vazões mássicas de óleo de soja bruto equivalentes a 11,488 ton¿h-1. Os fatores avaliados apresentaram efeito significativo sobre as dimensões calculadas, ao obterem-se diâmetros de coluna compreendidos entre 2,29 m e 2,94 m, bem como alturas de zona de extração entre 5,89 m e 69,07 m. Para sistemas compostos por óleos vegetais + ácidos graxos livres + etanol + água, os efeitos das variáveis operacionais de colunas mecanicamente agitadas sobre os perfis de tamanhos de gotas e de composições de fases são ainda pouco elucidados. Desta forma, este estudo revela-se de grande importância para a efetiva inserção dessa alternativa de processo no refino de óleos vegetais, ao proporcionar com que os métodos de design e scale up elevem-se a patamares quantitativamente mais precisos / Abstract: Deacidification of vegetable oils by liquid-liquid extraction seems to be an attractive alternative to high oil losses and energy costs typically found in alkali refining and by distillation of free fatty acids, respectively. The use of raw materials attained from renewable sources and the absence of residuals provides also a relevant environmental feature to the process. Descriptive models of phase composition profiles, based on drop population balances and multicomponent mass transfer, are essential for the development of design and scale up methods of liquid-liquid extraction columns. The major aim of this work was to evaluate correlations, methods and guidelines for sizing rotating disc columns applied to soybean oil deacidification. Equilibrium phase compositions, densities, viscosities and interfacial tensions for systems composed of soybean oil + commercial linoleic acid + ethanol + water at 298.2 K were experimentally determined using alcoholic solvents with water mass fractions of (5.00, 8.00, 11.00 and 14.00) %. The relative absolute deviations between experimental data and those calculated from empirical equations were lower than 6.36 %. Phase compositions profiles, quoted using 3 different models, were correlated to experimental data described in literature, determined in a rotating disc column (RDC) with 5.0 cm in diameter, which was used for corn oil deacidification. The relative absolute deviations between the free fatty acid mass fractions experimentally determined and those calculated from simulation were around 20 %. In a hypothetical study, rotating disc columns were sized for different operational conditions and water mass fractions in the solvent, considering crude soybean oil mass flow rates of 11.488 ton¿h-1. The studied factors were significant in the calculated dimensions, once the column diameters varied from (2.29 to 2.94) m and the column heights ranged from (5.89 to 69.07) m. For systems composed of vegetable oils + free fatty acids + ethanol + water, the effects of operational conditions of mechanically stirred columns on drop size and phase compositions profiles are still not well elucidated. Thus, this work becomes of great importance in the effective application of this alternative process in vegetable oils refining, shifting of column design and scale up methods to a quantitatively more precise level / Mestrado / Mestre em Engenharia de Alimentos
6

Techniques to Analyze Underdeposit Corrosion

Tinani, Suraj P. 20 July 2010 (has links)
No description available.
7

Extração da ascorbato oxidase de Cucurbita maxima por processo descontínuo e contínuo em coluna de discos rotativos perfurados utilizando sistemas de duas fases aquosas / Extraction of ascorbate oxidase from Cucurbita maxima by discontinuous and continuous process in perforated rotating disc contactor using aqueous two-phase systems.

Tatiana Souza Porto 21 May 2008 (has links)
A partição e purificação de ascorbato oxidase de abóbora (Cucurbita maxima) por extração líquido-líquido em sistema de duas fases aquosas (SDFA), pelos processos descontínuos e contínuos, utilizando coluna de discos rotativos perfurados (PRDC), foram estudadas. Foram utilizados planejamentos estatísticos para selecionar as variáveis significativas no processo descontínuo de purificação, e as variáveis estudadas foram massa molar e concentração do polietileno glicol (PEG), concentração de citrato, pH, concentração de NaCl, fator de diluição e massa total do sistema. Os melhores resultados (coeficiente de partição 1,72, recuperação 90,8% e aumento de pureza 3,12) foram obtidos nas seguintes condições: massa molar do PEG 20000 (g/mol), pH 6,0, concentração de PEG 25% (m/m) e concentração de citrato 10% (m/m). No valor de pH 6,0 e temperatura 35°C a ascorbato oxidase apresentou seus maiores valores de atividade, e manteve a estabilidade na faixa de pH 5,0 a 9,0 durante 36 horas e a temperaturas de até 40°C durante 1 hora. Experimentos também foram realizados para estimar as principais propriedades cinéticas e termodinâmicas da atividade e estabilidade da ascorbato oxidase, e esse estudo revelou que a enzima foi estável nas condições testadas. A PRDC mostrou um bom desempenho para extração da ascorbato oxidase em modo contínuo utilizando SDFA. A melhor condição operacional selecionada neste estudo foi selecionada com o auxílio de planejamentos estatísticos, sendo selecionadas as seguintes condições: massa molar do PEG 20000 (g/mol), concentração de PEG 20% (m/m), concentração de citrato 10% (m/m), velocidade de rotação dos discos de 80 rpm e velocidade da fase dispersa de 2 mL/min. Os melhores resultados em valores médios foram: coeficiente de partição 3,36, recuperação 152%, aumento de pureza 2,31, coeficiente de transferência de massa 0,045, eficiência de separação 43,7% e hold up 0,33. Os dados experimentais demonstram o potencial da aplicação do sistema de duas fases aquosas PEG/citrato para purificar a ascorbato oxidase utilizando coluna de discos rotativos perfurados. / The partition and purification of ascorbate oxidase from pumpkin (Cucurbita maxima) by liquid-liquid extraction in aqueous two-phase system (ATPS) by discontinuous and continuous process, using perforated rotating disc contactor (PRDC) was studied. Experimental designs were used to choose the significant variables for discontinuous process, and polyethylene glycol (PEG) molar mass and concentration, citrate concentration, pH, NaCl concentration, dilution factor and total mass of the system, were the variables studied. The better results (partition coefficient 1.72, recovery 90.8% and purification factor 3.12) were obtained with following conditions: PEG molar mass of 20000 g/mol, pH 6.0, PEG concentration of 25% (w/w) and citrate concentration of 10% (w/w). In the pH 6.0 and temperature of 35?C the ascorbate oxidase showed their high activity values and the enzyme was stable in the pH range of 5.0 to 9.0 during 36 hours and temperatures up to 40?C for 1 hour. Experiments were also conducted to estimate the main kinetic and thermodynamic properties of ascorbate oxidase activity and stability, and this study revealed the interesting stability of this enzyme. The PRDC showed a good performance for extracting in continuous mode using aqueous two-phase systems. The best operating condition was selected in this study for the extraction of ascorbate oxidase in the PRDC, and it was obtained with PEG molar mass of 20000 g/mol, PEG concentration of 20% (w/w) and citrate concentration of 10% (w/w), the disc rotational speed of 80 rpm and dispersed phase flowrate of 2 mL/min. The results in mean values were: partition coefficient 3.36, recovery 152%, purification factor 2.31, mass transfer coefficient 0.045, separation efficiency 43.7% and Hold up 0.33. The experimental data showed the potential application of aqueous two-phase systems PEG/citrate to purification ascorbate oxidase using perforated rotating disc contactor.
8

Extração da ascorbato oxidase de Cucurbita maxima por processo descontínuo e contínuo em coluna de discos rotativos perfurados utilizando sistemas de duas fases aquosas / Extraction of ascorbate oxidase from Cucurbita maxima by discontinuous and continuous process in perforated rotating disc contactor using aqueous two-phase systems.

Porto, Tatiana Souza 21 May 2008 (has links)
A partição e purificação de ascorbato oxidase de abóbora (Cucurbita maxima) por extração líquido-líquido em sistema de duas fases aquosas (SDFA), pelos processos descontínuos e contínuos, utilizando coluna de discos rotativos perfurados (PRDC), foram estudadas. Foram utilizados planejamentos estatísticos para selecionar as variáveis significativas no processo descontínuo de purificação, e as variáveis estudadas foram massa molar e concentração do polietileno glicol (PEG), concentração de citrato, pH, concentração de NaCl, fator de diluição e massa total do sistema. Os melhores resultados (coeficiente de partição 1,72, recuperação 90,8% e aumento de pureza 3,12) foram obtidos nas seguintes condições: massa molar do PEG 20000 (g/mol), pH 6,0, concentração de PEG 25% (m/m) e concentração de citrato 10% (m/m). No valor de pH 6,0 e temperatura 35°C a ascorbato oxidase apresentou seus maiores valores de atividade, e manteve a estabilidade na faixa de pH 5,0 a 9,0 durante 36 horas e a temperaturas de até 40°C durante 1 hora. Experimentos também foram realizados para estimar as principais propriedades cinéticas e termodinâmicas da atividade e estabilidade da ascorbato oxidase, e esse estudo revelou que a enzima foi estável nas condições testadas. A PRDC mostrou um bom desempenho para extração da ascorbato oxidase em modo contínuo utilizando SDFA. A melhor condição operacional selecionada neste estudo foi selecionada com o auxílio de planejamentos estatísticos, sendo selecionadas as seguintes condições: massa molar do PEG 20000 (g/mol), concentração de PEG 20% (m/m), concentração de citrato 10% (m/m), velocidade de rotação dos discos de 80 rpm e velocidade da fase dispersa de 2 mL/min. Os melhores resultados em valores médios foram: coeficiente de partição 3,36, recuperação 152%, aumento de pureza 2,31, coeficiente de transferência de massa 0,045, eficiência de separação 43,7% e hold up 0,33. Os dados experimentais demonstram o potencial da aplicação do sistema de duas fases aquosas PEG/citrato para purificar a ascorbato oxidase utilizando coluna de discos rotativos perfurados. / The partition and purification of ascorbate oxidase from pumpkin (Cucurbita maxima) by liquid-liquid extraction in aqueous two-phase system (ATPS) by discontinuous and continuous process, using perforated rotating disc contactor (PRDC) was studied. Experimental designs were used to choose the significant variables for discontinuous process, and polyethylene glycol (PEG) molar mass and concentration, citrate concentration, pH, NaCl concentration, dilution factor and total mass of the system, were the variables studied. The better results (partition coefficient 1.72, recovery 90.8% and purification factor 3.12) were obtained with following conditions: PEG molar mass of 20000 g/mol, pH 6.0, PEG concentration of 25% (w/w) and citrate concentration of 10% (w/w). In the pH 6.0 and temperature of 35?C the ascorbate oxidase showed their high activity values and the enzyme was stable in the pH range of 5.0 to 9.0 during 36 hours and temperatures up to 40?C for 1 hour. Experiments were also conducted to estimate the main kinetic and thermodynamic properties of ascorbate oxidase activity and stability, and this study revealed the interesting stability of this enzyme. The PRDC showed a good performance for extracting in continuous mode using aqueous two-phase systems. The best operating condition was selected in this study for the extraction of ascorbate oxidase in the PRDC, and it was obtained with PEG molar mass of 20000 g/mol, PEG concentration of 20% (w/w) and citrate concentration of 10% (w/w), the disc rotational speed of 80 rpm and dispersed phase flowrate of 2 mL/min. The results in mean values were: partition coefficient 3.36, recovery 152%, purification factor 2.31, mass transfer coefficient 0.045, separation efficiency 43.7% and Hold up 0.33. The experimental data showed the potential application of aqueous two-phase systems PEG/citrate to purification ascorbate oxidase using perforated rotating disc contactor.
9

Исследование окислительно-восстановительных превращений противовирусных веществ азоло-азинового ряда методами вольтамперометрии и ЭПР-спектроскопии : магистерская диссертация / Investigation of oxidation-reduction transformations of antiviral substances of the azolo-azine series by the methods of voltammetry and EPR spectroscopy

Баушева, А. В., Bausheva, A. V. January 2017 (has links)
Целью диссертационного исследования является изучение процессов восстановления нитрогруппы в препаратах азоло-азинового ряда с применением электрохимических методов и ЭПР-спектроскопии. Для достижения стабильных и воспроизводимых данных была разработана методика эксперимента. Рассмотрены вопросы электровосстановления фармпрепаратов содержащих нитрогруппу в своем строении и применение ЭПР – спектроскопии и электрохимических методов анализа, в частности вольтамперометрии, для установления механизма восстановления лекарственных веществ в теле человека. В ходе экспериментальной части установлена природа происходящих процессов, в том числе, природа лимитирующей стадии, проведен расчет количества электронов, принимающих участие в процессах электровосстановления основного вещества препаратов TRIAZAVIRIN® и TRIAZID®. Предложены вероятные механизмы протекания исследуемого процессов восстановления нитрогруппы исследуемых соединений. / The main substances of the newest Russian antiviral drugs, the aziolo-azine series TRIAZAVIRIN® and TRIAZID®, served as the research subjects. Objective: to study the processes of reduction of the nitro group in these compounds using electrochemical methods and EPR spectroscopy. An analysis of the literature data showed that the pharmaceutical activity of preparations containing a nitro group is due to its reduction. Electrochemical methods of analysis make it possible to study the in vitro transformation of the preparation as close as possible to the processes taking place with the drug in vivo. The method of EPR-spectroscopy allows obtaining reliable data on the free radical formed during the reaction, which can be a determining factor of the biological activity of the preparation. These methods were taken as a basis for studying the processes of nitro group reduction, which is a part of the basic substances of TRIAZAVIRIN® (TRZ) and TRIAZID® (TZ) preparations. The processes of nitro group reduction in TRZ and TZ molecules were studied using voltammetry and EPR spectroscopy. It has been established that the rate of reduction of the nitro group TRZ is controlled by diffusion, the process of reduction of the nitro group of the preparation is stepwise, irreversible and proceeds at a potential of -0.35 V through the formation of an anion radical with addition of 4e. It is shown that the rate of reduction of the nitro group of TZ is controlled by diffusion. The single-wave reduction process of the nitro group TZ at a potential of 6 -0.65 V is irreversible, goes through the formation of an anion radical with addition of 6e. Possible schemes for the recovery of the nitro group of the basic substances of TRIAZAVIRIN® and TRIAZID® preparations are proposed.

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