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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.
11

Development of methods for the analysis of petroleum contaminated soils

Okop, Imeh January 2010 (has links)
Soil contamination from petroleum spills is a frequent environmental problem in the world. It is obvious that petroleum exploration has contributed immensely to the economic growth of Nigeria, but over the last few decades, the Niger Delta of Nigeria has suffered grave human health risk and ecosystem degradation resulting from oil spillages, petroleum products leakages and other involuntary effluent discharges from oil exploration activities. This research seeks to develop and optimize GC-FID methods for the analysis of Petroleum hydrocarbons. Crude oil spillage contamination of soil from the Niger Delta was investigated 3 months after a crude oil-pipeline spillage. 47 Soil samples (300-500g) were collected at several points in the South-South Niger Delta. Control samples were taken from four unaffected sites within the vicinity of spillage with similar soil characteristics. Samples were collected at depths of 0-15 cm, 15-30 cm and 30-60 cm. The soil samples were prepared for analysis using solvent extraction methods, passed through column of sodium sulphate and Florisil® to aid in column performance, remove moisture and gross impurities. Samples were analysed using gas chromatography with a flame ionisation detector. Penetration and migration of C10-C26 and C26-C34 hydrocarbons through the soil layers were assessed by cluster analysis to determine the spatial distribution, penetration and chemical similarity of these compounds over the contaminated area. This information is a useful guide for bioremediation purpose. It was found that total petroleum hydrocarbon concentrations varied from 9-289 mgkg-1 topsoil, 8-318 mgkg-1 subsoil and 7-163 mgkg-1 at the greatest depth measured.The results show elevated levels of total hydrocarbon contents when compared with the reference sites. Drastic steps should be taken to carefully monitor and remediate the environment. Bioremediation with plants and micro-organisms is endorsed.
12

Výběr a optimalizace metody stanovení volných mastných kyselin / The selection and optimization of the method for assessment of free fatty acids

Koval, Dominik January 2018 (has links)
This master´s thesis deals with optimization and validation of method for determination of free fatty acids. The theoretical part is focused on possibilities of extraction, extract separation, esterification, gas chromatography determination and brief description of the most important validation parameters. All with main emphasis on applying on free fatty acids. The experimental part describes the selection and procedure of optimizing individual steps of the method. Extraction of lipids was performed by solvent mixture (diethylether/petroleumether), based on the standard ČSN EN ISO 1735, for the extraction of free fatty acid solid phase extraction was tested. The acid catalyzed esterification based on ČSN EN ISO 5509 using methanolic solution BF3 was used for derivatization of free fatty acids and a gas chromatograph with a flame ionization detector was used for their determination. Subsequently, selected validation parameters of the method were verified: repeatability, reproducibility, linearity, limits of detection and quantitation. Sunflower oil and emmental type cheese, bought in common food market, were used as model samples for selection and optimatization of the method.
13

Komplexní charakterizace plodů angreštu / Complex characterisation of gooseberry fruits

Rodzíková, Martina January 2014 (has links)
This thesis deals with the assessment of aroma active compounds in gooseberry and sensory analysis of it focusing on flavour. The theoretical part describes general characteristics, biological marks and properties of selected varieties, healing abilities, the active substances contained in gooseberry fruits and their use. The aim of the experimental part was to determine aroma-active substances contained in fruits of nineteen selected cultivars of gooseberry using SPME-GC-FID method. In total 45 volatile compounds were identified, among them 17 alcohols, 11 aldehydes, 6 ketones, 9 esters and 2 acids. For a better identification one sample (Captivátor variety) was also analysed using GC-MS with purge and trap extraction. Pentan-1-ol, hexanal, pentanal, ethylethanoate, ethylbutanoate, methylethanoate, methylbutanoate and ethanol were confirmed using mass spectra. Only several cultivars were selected for the assessment of overall sensory quality and palatability of fruits. Karmen and Remarka varieties were considered as the best samples by assessors.
14

Charakterizace plodů bezu černého / Characterisation of elderberry fruits

Christovová, Silvia January 2014 (has links)
This master's thesis deals with the characterization of elderberry fruit (Sambucus nigra L.) with emphasis on the aroma active compounds (AAC) and vitamin C (ascorbic acid (AA), dehydroascorbic acid (DHA)). The theoretical part gives a brief outlook on the chemical composition and attributes of Sambucus berries, its healing properties and the means of processing. The rest of the theoretical part thoroughly examines the AAC and vitamin C. The suitable assessment methods are also discussed. The experimental part of the work consists of two main tasks. The first one was to assess the aroma profile of Sambucus berries using the HS-SPME-GC-FID. 18 samples were examined (the wild elderberry and 17 cultivated varieties). In total, 24 different volatile aroma active compounds were identified and quantified, 12 of which belonged to alcohols, 5 to aldehydes, 4 to esters, 1 to acids and 2 “other” compounds (linalool and -damascenone). The chemical composition of the individual samples was not uniform; no single sample contained all of the identified compounds. The second task was to assess the total vitamin C content (the sum of DHA and AA) using the HPLC. For the purpose of reducing DHA to AA three reducing agents were examined (DTT, TCEP and L-cysteine) at two different pH levels (7 and 4). TCEP at pH 4 turned out to be most efficient and was subsequently applied on the samples of 5 selected elderberry varieties. The measured vitamin C content was within the range of 5,1 – 13,0 mg per 100 g of fruit.
15

Změny obsahu mastných kyselin během výroby modelového sýra / Changes of fatty acids during production of model cheese

Janoušková, Kateřina January 2017 (has links)
This thesis deals with the identification and quantification of free and bound fatty acids in model cheese samples of the Moravský bochník type, which were produced at Tomas Bata University in Zlín by a standard technological procedure. In a theoretical part of the thesis, the issues of lipids, fatty acids, as well as the characteristics of high cooked cheeses including Moravský bochník, microbial cultures used in their production, and the possibilities of fatty acids determination are summarized. The ČSN EN ISO 1735:2005 method was chosen for the lipid extraction from cheese samples. Present free and bound fatty acids were identified and quantified by gas chromatography with flame-ionization detection after conversion to methylesters by acid esterification with bortrifluoride as a catalyst. In total 32 fatty acids were identified in cheese samples, the highest amount of caproic, caprylic, capric, lauric, myristic, palmitic, stearic and oleic acids.
16

Extratos vegetais amazônicos no processo têxtil: caracterização físico-química e aplicações / Amazonian plant extracts on textile process : physicochemical characterization and application

Leonardi, Bárbara 15 February 2016 (has links)
Os extratos vegetais amazônicos para uso em beneficiamento têxtil podem ser uma alternativa sustentável e ecológica em relação às atuais matérias-primas utilizadas pelo mercado. Este estudo teve como objetivo efetuar a caracterização físicoquímica de extratos vegetais amazônicos (óleo-resina de copaíba, óleo de castanha do Brasil, óleo de buriti, manteiga de cacau, manteiga de tucumã e manteiga de cupuaçu), preparar emulsões e realizar aplicações preliminares destas em têxteis. A caracterização físico-química foi realizada através das técnicas instrumentais analíticas de espectroscopia de infravermelho por transformada de Fourrier (FTIR) e cromatografia a gás com detecção por ionização de chama (CG-FID). Além disso, foi realizada a determinação do Equilíbrio Hidrófilo-Lipófilo (EHL) das emulsões preparadas a partir dos extratos estudados; seleção da emulsão mais estável por extrato para aplicação por foulardagem; avaliação da oxidação das emulsões aplicadas sobre o material têxtil em diferentes temperaturas (120 a 200ºC); e avaliação sensorial de toque proporcionado pelas emulsões em comparação a um amaciante de uso industrial. Os principais resultados foram que o óleo de castanha do Brasil e as manteigas de cacau, tucumã e cupuaçu apresentaram resultados próximos nas análises por FTIR; a distribuição graxa por cromatografia a gás mostrou-se útil para a caracterização destes extratos vegetais; os valores de referência de EHL para os extratos analisados foram de 7,51 a 10,72 e estão de acordo com a literatura científica (de 6 a 12); os extratos estudados emulsionados nas condições do estudo não possuem tendência à oxidação por temperatura; as médias globais das análises sensoriais de toque indicam um resultado inferior ao padrão comercial, porém, as manteigas de cacau, cupuaçu e o óleo de castanha do Brasil apresentaram os melhores resultados, com notas entre 2,8 e 2,9 (numa escala de 1 a 5). Assim, nota-se que, os resultados obtidos podem ser utilizados como base para pesquisas futuras no sentido de melhorar as formulações das emulsões para a produção de amaciantes ou outros produtos / The Amazonian plant extracts for use in textile processing can be a sustainable and environmentally friendly alternative to the current raw materials used by the market. This study aimed to make the physicochemical characterization of Amazonian plant extracts (copaiba oleoresin, Brazil nut oil, buriti oil, cocoa butter, tucumã butter and cupuaçu butter), prepare emulsions and perform preliminary applications in textile. The physicochemical characterization was performed by analytical instrumental techniques, such as FTIR spectroscopy and gas chromatography with FID detection (GC-FID). Furthermore, the determination of the Hydrophile-Lipophile Balance (HLB) was performed of the emulsions prepared from the extracts studied; the emulsion more stable for selection extract for application by padding; evaluation of the oxidation of emulsions applied to the textile material at different temperatures (120 to 200C); and sensory evaluation provided by the touch emulsions compared to a industrial softener. The main results were that the Brazil nut oil and cocoa, tucumã and cupuaçu butters showed similar results in the analysis by FTIR; grease distribution by gas chromatography proved to be useful for the characterization of plant extracts; the HLB values for the reference analyzed the extracts were 7.51 to 10.72 are consistent with the literature (6 to 12); the extracts studied emulsified in the study conditions have no tendency to oxidation temperature; the global average of sensory analysis touch indicate somewhat lower than the commercial standard, however, cocoa and cupuaçu butter and Brazil nut oil showed the best results, with grades between 2.8 and 2.9 (on a scale of 1 to 5). Thus, it is noted that the results obtained can be used as the basis for further research in order to improve the formulations of emulsions for the production of fabric softeners or other products
17

Extratos vegetais amazônicos no processo têxtil: caracterização físico-química e aplicações / Amazonian plant extracts on textile process : physicochemical characterization and application

Bárbara Leonardi 15 February 2016 (has links)
Os extratos vegetais amazônicos para uso em beneficiamento têxtil podem ser uma alternativa sustentável e ecológica em relação às atuais matérias-primas utilizadas pelo mercado. Este estudo teve como objetivo efetuar a caracterização físicoquímica de extratos vegetais amazônicos (óleo-resina de copaíba, óleo de castanha do Brasil, óleo de buriti, manteiga de cacau, manteiga de tucumã e manteiga de cupuaçu), preparar emulsões e realizar aplicações preliminares destas em têxteis. A caracterização físico-química foi realizada através das técnicas instrumentais analíticas de espectroscopia de infravermelho por transformada de Fourrier (FTIR) e cromatografia a gás com detecção por ionização de chama (CG-FID). Além disso, foi realizada a determinação do Equilíbrio Hidrófilo-Lipófilo (EHL) das emulsões preparadas a partir dos extratos estudados; seleção da emulsão mais estável por extrato para aplicação por foulardagem; avaliação da oxidação das emulsões aplicadas sobre o material têxtil em diferentes temperaturas (120 a 200ºC); e avaliação sensorial de toque proporcionado pelas emulsões em comparação a um amaciante de uso industrial. Os principais resultados foram que o óleo de castanha do Brasil e as manteigas de cacau, tucumã e cupuaçu apresentaram resultados próximos nas análises por FTIR; a distribuição graxa por cromatografia a gás mostrou-se útil para a caracterização destes extratos vegetais; os valores de referência de EHL para os extratos analisados foram de 7,51 a 10,72 e estão de acordo com a literatura científica (de 6 a 12); os extratos estudados emulsionados nas condições do estudo não possuem tendência à oxidação por temperatura; as médias globais das análises sensoriais de toque indicam um resultado inferior ao padrão comercial, porém, as manteigas de cacau, cupuaçu e o óleo de castanha do Brasil apresentaram os melhores resultados, com notas entre 2,8 e 2,9 (numa escala de 1 a 5). Assim, nota-se que, os resultados obtidos podem ser utilizados como base para pesquisas futuras no sentido de melhorar as formulações das emulsões para a produção de amaciantes ou outros produtos / The Amazonian plant extracts for use in textile processing can be a sustainable and environmentally friendly alternative to the current raw materials used by the market. This study aimed to make the physicochemical characterization of Amazonian plant extracts (copaiba oleoresin, Brazil nut oil, buriti oil, cocoa butter, tucumã butter and cupuaçu butter), prepare emulsions and perform preliminary applications in textile. The physicochemical characterization was performed by analytical instrumental techniques, such as FTIR spectroscopy and gas chromatography with FID detection (GC-FID). Furthermore, the determination of the Hydrophile-Lipophile Balance (HLB) was performed of the emulsions prepared from the extracts studied; the emulsion more stable for selection extract for application by padding; evaluation of the oxidation of emulsions applied to the textile material at different temperatures (120 to 200C); and sensory evaluation provided by the touch emulsions compared to a industrial softener. The main results were that the Brazil nut oil and cocoa, tucumã and cupuaçu butters showed similar results in the analysis by FTIR; grease distribution by gas chromatography proved to be useful for the characterization of plant extracts; the HLB values for the reference analyzed the extracts were 7.51 to 10.72 are consistent with the literature (6 to 12); the extracts studied emulsified in the study conditions have no tendency to oxidation temperature; the global average of sensory analysis touch indicate somewhat lower than the commercial standard, however, cocoa and cupuaçu butter and Brazil nut oil showed the best results, with grades between 2.8 and 2.9 (on a scale of 1 to 5). Thus, it is noted that the results obtained can be used as the basis for further research in order to improve the formulations of emulsions for the production of fabric softeners or other products
18

Produção de biodiesel empregando biocatálise via reações de esterificação e transesterificação / Biodiesel production employing biocatalysis by esterification and transesterification reactions

Rosset, Isac George 14 March 2011 (has links)
Neste trabalho prepararam-se ésteres de ácidos graxos por esterificação do ácido oléico e transesterificação do óleo de soja e do triéster oléico via catálise enzimática. Determinou-se a composição dos produtos obtidos por RMN 1H e CG-FID. Os padrões dos ésteres do ácido oléico via esterificação ácida foram preparados empregando ácido sulfúrico, os padrões dos ésteres do óleo de soja por transesterificação básica com hidróxido de sódio e o padrão do triéster oléico foi sintetizado utilizando ácido p-tolueno sulfônico como catalisador. A melhor enzima para essas reações foi determinada através de reações de esterificação do ácido oléico e transesterificação do óleo de soja com etanol na ausência de co-solventes, sendo que foi selecionada a lipase de Candida antarctica. A mesma enzima foi empregada nas esterificações enzimáticas do ácido oléico com diversos alcoóis (metanol, etanol, n-propanol e n-butanol), na transesterificação enzimática do óleo de soja e do triéster oléico com etanol. Em ambos os estudos, foram avaliados os fatores que influenciam as reações: quantidade de enzima; tempo de reação; água adicionada ao álcool e reuso do biocatalisador. Na esterificação enzimática do ácido oléico, o uso do etanol forneceu o melhor rendimento (96,5%) com 5,0% (m/m) de enzima em 24 horas de reação. Quando uma quantidade de 4,0% de água foi adicionada ao álcool, a reação utilizando metanol mostrou maior eficiência (98,5%) e os rendimentos com os outros alcoóis não foram alterados significativamente (acima de 90%). Também foi possível utilizar a enzima por até 10 ciclos sem perda de rendimento, com exceção do metanol, onde ocorreu um decréscimo acentuado de rendimentos nos ciclos seguintes. Na transesterificação enzimática do óleo de soja, os mesmos fatores foram avaliados e com 5,0% de enzima, após 24 horas, foi obtido um rendimento de 84,1% e com a adição de água o rendimento não foi significativamente alterado (83%). Na transesterificação, os métodos de quantificação por RMN 1H e CG-FID foram comparados sendo que uma maior diferença foi observada para as reações com baixos rendimentos por RMN 1H, porém em altos rendimentos a diferença entre os dois métodos não foi significativa. Monoglicerídeos e diglicerídeos foram quantificados por CG-FID e por RMN 1H onde foi possível calcular a razão dos produtos formados através de uma equação desenvolvida, sendo que a diferença entre esses tipos de análises foi pequena, de apenas 1,4%. A transesterificação enzimática do triéster oléico foi obtida em bom rendimento (90,4%) e uma pequena quantidade de mono- e diglicerídeos foi produzida. Em todas as reações de transesterificação, o glicerol não foi detectado após a lavagem dos produtos. A metodologia empregando a lipase de Candida antarctica mostrou-se eficiente para a produção de biodiesel a partir do óleo de soja e do ácido oléico com diferentes tipos de alcoóis. / In this work, it was prepared esters of the fatty acid by esterification of the oleic acid and transesterification of the soy oil through enzymatic catalysis. It was determined the composition of the products obtained by 1H NMR and GC-FID. The standards of esters of the oleic acid by acid esterification was prepared employing sulfuric acid, the standards of esters of the soy oil by alkaline transesterification with sodium hydroxide and the standard of the oleic triester was synthesized employing p-toluene sulfonic acid as catalyst. The best enzyme for those reactions was determined through reactions of esterification of the oleic acid and transesterification of the soy oil with ethanol and free co-solvents, and lipase from Candida antarctica was selected. The same enzyme was employed in the enzymatic esterifications of the oleic acid with various alcohols (methanol, ethanol, propanol and butanol), in the enzymatic transesterification of soy oil and the oleic triester with ethanol. In both studies, was assessed the factors that influence the reactions: amount of catalyst, reaction time, water added in the alcohol and the turnover of biocatalyst. In the enzymatic esterification of the oleic acid, the ethanol showed the better yield (96,5%) with 5,0% (m/m) of enzyme at 24 hours of reaction. When 4,0% of water was added to the alcohol, the methanol showed the high efficiency (98,5%) and the yield with another alcohols were not affected. It was also possible to use the enzyme for 10 cycles without lose yield, except for the methanol. In the enzymatic transesterification of the soy oil, the same factors were assessed using 5,0% of enzyme, after 24 hours, a yield of 84,1% was obtained and with the water addition the yield was not modified (83%). On the transesterification, 1H NMR and GC-FID were compared and a great difference was observed for low yields, but on high yields, the difference between methods was small. Monoglycerides and diglycerides were quantified by GC-FID and detected by 1H NMR, it was possible to calculate the ratio between them on the products formed through an equation developed and the difference for this type of analysis was small, only 1.4% . The enzymatic transesterification of the oleic triester was obtained with good yield (90,4%) and a small amount of the monoglycerides and diglycerides was produced. In all the transesterifications reactions, glycerol was not detected after washing mixture of products. The methodology employing Candida antarctica lipase was efficient for biodiesel production by soybean oil and oleic acid with different alcohols.
19

COMPOSTOS VOLÁTEIS E PARÂMETROS DE QUALIDADE DE DIFERENTES GENÓTIPOS DE FRUTOS DE BUTIA ODORATA. / VOLATILE COMPOUNDS AND QUALITY PARAMETERS FROM DIFFERENT GENOTYPES OF BUTIA ODORATA.

Ferrão, Tassiane dos Santos 27 February 2012 (has links)
The Butia odorata has received special attention from the scientific community because of their nutritional and functional properties that have been revealed, in addition to its rightdown sensory characteristics. The aim of this study was to characterize different genotypes from Butia odorata fruit collected in Santa Maria - RS (SM) and Santa Rosa - RS (SR) regions during three consecutive harvests in relation to various physical and chemical properties. Many analyses were performed like: biometric, color and quality parameters, fatty acid composition in the Butia pulp. An HS-SPME method was developed for the isolation and subsequent quantification (GC-FID) and identification (GC/MS) of volatile compounds (VCs). The biometric parameters results showed pulp yields between 40.38 and 73.91%. The color of the pulp ranged between yellow and orange shades. TSS ranged between 12.39 and 15.50 °Brix, acidity between 0.69 and 2.26 g% citric acid and pH between 3.17 and 3.95. The fruit had humidity between 78.04 and 85.85 g%; ashes between 0.47 and 0.77 g%; protein between 0.57 and 0.93 g%, crude fiber between 0.84 and 4.02 g%; lipid between 0.12 and 2.27 g%. The fatty acids such as palmitic acid, linoleic and linolenic acids were found in abundance. It was possible to observe the partial discrimination between the two regions in the PCA using the physico-chemical variables. The samples from SR characterized by high scores for lipids and palmitic acid, while SM samples showed a higher humidity and TSS. The method employed use DVB/CAR/PDMS fiber for the VCs extraction of the centrifuged Butia pulp , added with 30% NaCl, and maintaining the system at a temperature of 35 °C for 45 minutes, under stirring. The volatile fraction was analyzed in GC and were identified 77 compounds among acids (5), alcohols (14), aldehydes (9), ketones (12), lactones (3), terpenes (2) and esters (34). The ethyl hexanoate compound was the major compound in almost samples. The PCA from VCs enabled to realize grouping of samples into two groups according to region of origin. The fruits from Santa Maria showed a high content of esters and the fruits from Santa Rosa had higher concentrations of alcohols and aldehydes. An exploratory analysis of the variables of physico-chemical composition and volatile of the samples was observed using PCA. In the graphs analysis also realized a partial separation of samples according to their region: the samples SM2-10 and RS1-11 distanced themselves from the other and it indicates greater particularity in their chemical compositions. Therefore the fruits (Butia odorata) showed great variability in biometric characteristics, physico-chemical and volatile profiles according to region of origin. It indicates a strong influence of soil and climatic factors. In this study, the nutritional characteristics and high yield pulp of some Butia fruits demonstrated the high potential for fresh consumption or for the manufacture of processed products / O butiá (Butia odorata) tem recebido especial atenção da comunidade científica, em virtude de suas propriedades nutritivas e funcionais que estão sendo reveladas, além das suas características sensoriais peculiares, ainda pouco exploradas. Desta forma, o objetivo do presente trabalho foi caracterizar diferentes genótipos de frutos de butiazeiros coletados nas regiões de Santa Maria RS (SM) e Santa Rosa RS (SR) em três safras consecutivas, quanto as diversas propriedades físicoquímicas. Foram realizadas análises biométricas, de cor, dos parâmetros de qualidade, composição centesimal e ácidos graxos da polpa do butiá, além do desenvolvimento de método de isolamento por SPME com posterior quantificação (GC-FID) e identificação (GC/MS) dos compostos voláteis (CVs). Os resultados dos parâmetros biométricos revelaram rendimentos de polpa, entre 40,38 e 73,91%. A cor da polpa oscilou em tons de amarelo e laranja. Os SST variaram entre 12,39 e 15,50 °Brix, a acidez entre 0,69 e 2,26 g% em ácido cítrico e o pH entre 3,17 e 3,95. As frutas apresentaram umidade entre 78,04 e 85,85 g%; cinzas entre 0,47 e 0,77 g%, proteína entre 0,57 e 0,93 g%, fibra bruta entre 0,84 e 4,02 g% e lipídios de 0,12 a 2,27 g%. Os ácidos graxos encontrados em maior abundância foram o ácido palmítico, linoléico e linolênico. Na Análise dos Componentes Principais (PCA) empregando as variáveis físico-químicas observou-se a discriminação parcial entre as duas regiões, sendo as amostras da região de SR caracterizadas por elevados escores para lipídios e ácido palmítico, enquanto que as da região de SM apresentaram, em geral, maior umidade e teor de SST. O método desenvolvido emprega o uso da fibra DVB/CAR/PDMS para a extração dos CVs da polpa de butiá centrifugada, adicionada de 30% de NaCl, e mantendo o sistema a uma temperatura de 35 ºC por 45 minutos, sob agitação. A fração volátil foi analisada em GC e nela identificados 77 compostos entre ácidos (5), alcoóis (14), aldeídos (9), cetonas (12), lactonas (3), terpenos (2) e, principalmente, ésteres (34). Entre estes se destacou o hexanoato de etila como composto majoritário. A PCA dos CVs possibilitou ver o agrupamento das amostras em dois grupos conforme a região de origem, onde, em geral, os butiás de Santa Maria apresentaram elevado teor de ésteres, enquanto os de Santa Rosa obtiveram maiores concentrações de alcoóis e aldeídos. Uma análise exploratória entre as variáveis de composição físico-química e volátil das amostras estudadas foram observadas através de uma PCA. Na visualização dos gráficos notou-se também uma parcial separação das amostras quanto à região de origem, sendo que as amostras SM2-10 e SR1-11 distanciaram-se das demais, indicando maior particularidade em suas composições químicas. Sendo assim, os butiás apresentaram grande variabilidade em suas características biométricas, físicoquímicas e nos perfis voláteis em função da região de origem e safra e, portanto, apresentou forte influência de fatores edafoclimáticos. Sobretudo, as características nutricionais e o alto rendimento de polpa de alguns frutos de butiás evidenciaram, neste estudo, o alto potencial para consumo in natura ou mesmo para a fabricação de produtos processados.
20

Produção de biodiesel empregando biocatálise via reações de esterificação e transesterificação / Biodiesel production employing biocatalysis by esterification and transesterification reactions

Isac George Rosset 14 March 2011 (has links)
Neste trabalho prepararam-se ésteres de ácidos graxos por esterificação do ácido oléico e transesterificação do óleo de soja e do triéster oléico via catálise enzimática. Determinou-se a composição dos produtos obtidos por RMN 1H e CG-FID. Os padrões dos ésteres do ácido oléico via esterificação ácida foram preparados empregando ácido sulfúrico, os padrões dos ésteres do óleo de soja por transesterificação básica com hidróxido de sódio e o padrão do triéster oléico foi sintetizado utilizando ácido p-tolueno sulfônico como catalisador. A melhor enzima para essas reações foi determinada através de reações de esterificação do ácido oléico e transesterificação do óleo de soja com etanol na ausência de co-solventes, sendo que foi selecionada a lipase de Candida antarctica. A mesma enzima foi empregada nas esterificações enzimáticas do ácido oléico com diversos alcoóis (metanol, etanol, n-propanol e n-butanol), na transesterificação enzimática do óleo de soja e do triéster oléico com etanol. Em ambos os estudos, foram avaliados os fatores que influenciam as reações: quantidade de enzima; tempo de reação; água adicionada ao álcool e reuso do biocatalisador. Na esterificação enzimática do ácido oléico, o uso do etanol forneceu o melhor rendimento (96,5%) com 5,0% (m/m) de enzima em 24 horas de reação. Quando uma quantidade de 4,0% de água foi adicionada ao álcool, a reação utilizando metanol mostrou maior eficiência (98,5%) e os rendimentos com os outros alcoóis não foram alterados significativamente (acima de 90%). Também foi possível utilizar a enzima por até 10 ciclos sem perda de rendimento, com exceção do metanol, onde ocorreu um decréscimo acentuado de rendimentos nos ciclos seguintes. Na transesterificação enzimática do óleo de soja, os mesmos fatores foram avaliados e com 5,0% de enzima, após 24 horas, foi obtido um rendimento de 84,1% e com a adição de água o rendimento não foi significativamente alterado (83%). Na transesterificação, os métodos de quantificação por RMN 1H e CG-FID foram comparados sendo que uma maior diferença foi observada para as reações com baixos rendimentos por RMN 1H, porém em altos rendimentos a diferença entre os dois métodos não foi significativa. Monoglicerídeos e diglicerídeos foram quantificados por CG-FID e por RMN 1H onde foi possível calcular a razão dos produtos formados através de uma equação desenvolvida, sendo que a diferença entre esses tipos de análises foi pequena, de apenas 1,4%. A transesterificação enzimática do triéster oléico foi obtida em bom rendimento (90,4%) e uma pequena quantidade de mono- e diglicerídeos foi produzida. Em todas as reações de transesterificação, o glicerol não foi detectado após a lavagem dos produtos. A metodologia empregando a lipase de Candida antarctica mostrou-se eficiente para a produção de biodiesel a partir do óleo de soja e do ácido oléico com diferentes tipos de alcoóis. / In this work, it was prepared esters of the fatty acid by esterification of the oleic acid and transesterification of the soy oil through enzymatic catalysis. It was determined the composition of the products obtained by 1H NMR and GC-FID. The standards of esters of the oleic acid by acid esterification was prepared employing sulfuric acid, the standards of esters of the soy oil by alkaline transesterification with sodium hydroxide and the standard of the oleic triester was synthesized employing p-toluene sulfonic acid as catalyst. The best enzyme for those reactions was determined through reactions of esterification of the oleic acid and transesterification of the soy oil with ethanol and free co-solvents, and lipase from Candida antarctica was selected. The same enzyme was employed in the enzymatic esterifications of the oleic acid with various alcohols (methanol, ethanol, propanol and butanol), in the enzymatic transesterification of soy oil and the oleic triester with ethanol. In both studies, was assessed the factors that influence the reactions: amount of catalyst, reaction time, water added in the alcohol and the turnover of biocatalyst. In the enzymatic esterification of the oleic acid, the ethanol showed the better yield (96,5%) with 5,0% (m/m) of enzyme at 24 hours of reaction. When 4,0% of water was added to the alcohol, the methanol showed the high efficiency (98,5%) and the yield with another alcohols were not affected. It was also possible to use the enzyme for 10 cycles without lose yield, except for the methanol. In the enzymatic transesterification of the soy oil, the same factors were assessed using 5,0% of enzyme, after 24 hours, a yield of 84,1% was obtained and with the water addition the yield was not modified (83%). On the transesterification, 1H NMR and GC-FID were compared and a great difference was observed for low yields, but on high yields, the difference between methods was small. Monoglycerides and diglycerides were quantified by GC-FID and detected by 1H NMR, it was possible to calculate the ratio between them on the products formed through an equation developed and the difference for this type of analysis was small, only 1.4% . The enzymatic transesterification of the oleic triester was obtained with good yield (90,4%) and a small amount of the monoglycerides and diglycerides was produced. In all the transesterifications reactions, glycerol was not detected after washing mixture of products. The methodology employing Candida antarctica lipase was efficient for biodiesel production by soybean oil and oleic acid with different alcohols.

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