109 f. / Submitted by Ana Hilda Fonseca (anahilda@ufba.br) on 2013-04-03T13:32:48Z No. of bitstreams: 2 Pag_Iniciais.doc: 792576 bytes, checksum: 12dfaef31d9159988f77ea8619fd118e (MD5) Cap. I - V.doc: 4237312 bytes, checksum: be8dd2f149baada6ca89d1396f98bbb5 (MD5) / Rejected by Ana Hilda Fonseca(anahilda@ufba.br), reason: Solicito o envio em arquivo único. Transformar o arquivo em pdf sem senha. on 2013-04-18T16:41:59Z (GMT) / Submitted by Ana Hilda Fonseca (anahilda@ufba.br) on 2013-05-20T15:50:31Z No. of bitstreams: 1 Tese Luiz Souza Carvalho.pdf: 2954132 bytes, checksum: 0bd3a51a7e2edab66b3681ac3f94951f (MD5) / Approved for entry into archive by Ana Hilda Fonseca(anahilda@ufba.br) on 2013-05-20T15:51:43Z (GMT) No. of bitstreams: 1 Tese Luiz Souza Carvalho.pdf: 2954132 bytes, checksum: 0bd3a51a7e2edab66b3681ac3f94951f (MD5) / Made available in DSpace on 2013-05-20T15:51:43Z (GMT). No. of bitstreams: 1 Tese Luiz Souza Carvalho.pdf: 2954132 bytes, checksum: 0bd3a51a7e2edab66b3681ac3f94951f (MD5) Previous issue date: 2008 / CAPES / Os metais traço e os hidrocarbonetos policíclicos aromáticos particulados transportados por via aérea são considerados como um risco á saúde e ao ambiente, pois podem ser absorvido pelo tecido do pulmão humano durante a respiração. A queima de combustível fóssil e da madeira, assim como a incineração de dejetos e processos industriais, são as principais fontes antrópicas de metais e hidrocarbonetos policíclicos aromáticos (PAH) á atmosfera.. Este trabalho tem a finalidade de determinar as concentrações em suspensão (TSP e PM10 de metais, assim como as concentrações e os perfis dos 16 PAH prioritários para estudos ambientais segundo a U.S. EPA), que estão agregados ao material particulado. Os metais: Fe, Mn, Cu e Zn determinados por ICP-OES, e os PAH foram separados por cromatografia gasosa, identificados e quantificados por GC-MS. A amostragem foi feita em três sítios em Salvador-BA: i) Estação de ônibus da Lapa, ii) Porto de Aratu, iii) Vila de Bananeira,,na ilha de Maré próximo ao Porto de Aratu. Os dados experimentais foram analisados usando o programa (STATISTICA 6 Stat Soft). Para os metais: Fe apresentou as concentrações mais elevadas (variou de 26,8 a 328µgm-3) na maioria dos sítios, exceto bananeiras, onde o Zn predominou (variou de 1,83 a 145µgm-3). Para os hidrocarbonetos policíclicos aromáticos: BbF apresentou maiores concentrações na maioria dos sítios (variou de 0,130 a 6850ng m-3), exceto na estação da Lapa, predominou CRY(variou de 0,075 a 6,85µgm-3). Os metais e PAH, são principalmente de fonte antrópica, e podem originar sérios problemas de saúde / Salvador

Submitted by Ana Hilda Fonseca (anahilda@ufba.br) on 2016-05-02T15:47:06Z No. of bitstreams: 1 Dissertação_Larissa_corrigidaII.pdf: 1019512 bytes, checksum: edf232cf9ac3bc5e1e6b995c18e3398e (MD5) / Approved for entry into archive by Ana Hilda Fonseca (anahilda@ufba.br) on 2016-05-13T14:13:08Z (GMT) No. of bitstreams: 1 Dissertação_Larissa_corrigidaII.pdf: 1019512 bytes, checksum: edf232cf9ac3bc5e1e6b995c18e3398e (MD5) / Made available in DSpace on 2016-05-13T14:13:08Z (GMT). No. of bitstreams: 1 Dissertação_Larissa_corrigidaII.pdf: 1019512 bytes, checksum: edf232cf9ac3bc5e1e6b995c18e3398e (MD5) / CNPq / Alimentos industrializados, tais como misturas de condimento e sopas instantâneas, geralmente possuem alto teor salino em sua composição, o que torna mais difícil a quantificação dos micro elementos por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES). Nesse contexto, o presente trabalho teve como objetivo o estudo de estratégias para a determinação de elementos essenciais e não essenciais em matrizes alimentícias com alto teor salino por ICP OES. O estudo das variáveis potência de radiofrequência (PR) e vazão de gás de nebulização (VGN) foi realizado utilizando planejamento fatorial completo 22e matriz Doehlert. A partir da avaliação dos gráficos de superfície e dos perfis de desejabilidade, foi possível estabelecer uma condição operacional ótima de potência e vazão de 1250 We 1,0 L min-1, respectivamente. Foi também realizada a avaliação dos elementos Be, Ga, In, Sc e Y como candidatos a padrão interno. Esse estudo foi feito a partir da comparação dos coeficientes angulares de curvas analíticas preparadas na ausência, na presença da matriz, sem e com adição do padrão interno.Os candidatos recomendados foram Sc e Y. As amostras adquiridas em supermercados da cidade de Salvador, Bahia, foram submetidas ao procedimento de decomposição ácida assistida por radiação micro-ondas, cujas condições foram selecionadas com base no teor de carbono residual, na acidez residual e nas concentrações dos elementos de interesse. Os parâmetros de desempenho do método proposto foram estabelecidos com base nos limites de detecção e quantificação, teste de adição e recuperação, precisão e exatidão. A exatidão do método foi avaliada a partir da análise do material de referência certificado NIST 1570a (Trace Elements in Spinach Leaves) e foram obtidos percentuais de recuperação na faixa entre 84,4 a 104,4%. O método proposto foi aplicado em amostras com diferentes sabores de misturas de condimento e de sopas instantâneas. As faixas de concentração para os elementos determinados, em µg g-1, foram: Ba (0,312 – 1,865), Ca (348 - 3909); Cu (0,530 – 1,315); Fe (6,1 – 44,8); K (405 - 16403); Mg (97 - 504); Mn (0,504 – 8,416); P (332 – 2921), Sr (0,98 – 20,47), Zn (0,439 – 19,47) e em % m m-1 Na (2,84 – 10,21). Um estudo de acessibilidade “in vitro” nas amostras de sopas instantâneas foi realizado por meio do método in vitro SBET (Simple Bioaccessibility Extraction Test) e foi encontrada uma faixa de 7,5 – 87,1%, sendo a maior porcentagem para o elemento K. A contribuição deste trabalho está relacionada a proposta de novas estratégias que viabilizaram a avaliação da composição em termos de elementos essenciais em alimentos com alto teor salino. Além disso, informações inéditas foram obtidas sobre a acessibilidade para as amostras de sopas instantâneas. / Processed foods, such as seasonings mixtures and instant soups, usually have high salt levels in their composing which makes it more difficult quantification of microelements by inductively coupled plasma optical emission spectrometry (ICP OES). In this context, the present work had as objective the study of strategies for the determination of essential and non-essential elements in food matrices with high saline content by ICP OES. The study of radiofrequency power variables and nebulizer gas flow had performed using full 22 factorial design and Doehlert matrix. From the evaluation of surface charts and desirability profiles, it was possible to establish a suitable operating condition of 1250 W and 1.0 L min-1 for radiofrequency power and nebulizer gas flow, respectively. It was also performed the assessment of the elements Be, Ga, In, Sc and Y as candidates for internal standardization. This study was done from the comparison of the slope of analytical curves prepared in the absence, in the presence of the matrix, with and without addition of internal standard. The recommended candidates were Sc and Y. Samples purchased at supermarkets in the city of Salvador, Bahia, underwent the procedure of microwave-assisted acid decomposition, whose conditions were selected based on the residual carbon content, on residual acidity and on the concentrations of the elements of interest. The performance parameters of the proposed method were established based on limits of detection and quantification, addition and recovery testing, precision and accuracy. The accuracy of the method was evaluated from the analysis of certified reference material NIST 1570a (Trace elements in spinach leaves) and the recovery percentages were in the range between 84.4 to 104.4%. The proposed method was applied to samples with different flavors of seasoning mixtures and instant soups and the concentration ranges for certain elements, in µg g-1 were: Ba (0.312 – 1.865), Ca (348 – 3909); Cu (0.530 –1.315); Fe (6.1 –44.8); K (405 – 16403); Mg (97 – 504); Mn (0.504 – 8.416); P (332 –2921), Sr (0.98 – 20.47), Zn (0.439 – 19.47) and in% m m- 1Na (2.84 – 10.21). A study of accessibility in the samples of instant soups was done through the in vitro SBET method (Simple Bioaccessibility Extraction Test) and was found a range of 7.5 – 87.1%, being the largest value for the element K. The contribution of this work is related to proposed new strategies that enable the assessment of the composition in terms of essential elements in foods with high salt content. In addition, unpublished information was obtained about the accessibility for samples of instant soup

Made available in DSpace on 2016-06-02T20:35:09Z (GMT). No. of bitstreams: 1 TeseMCS.pdf: 2092312 bytes, checksum: 9994cc8bab5cc486586caf4f13ce51cf (MD5) Previous issue date: 2006-03-03 / Universidade Federal de Minas Gerais / The main goal of this thesis was the investigation of alternative procedures for chemical analysis of refractory materials and clays using an inductively coupled plasma optical emission spectrometry (ICP OES) with axial view by direct analysis of slurries and microwave-assisted alkaline digestion. The preliminary experiments of this work focused the introduction of slurries into the ICP OES with axial view and evaluated the effects caused by the particle size distribution on the intensities emission signals. Afterwards, a grinding method in which solid samples were ground together with chemical modifiers was developed. The chemical modifiers studied were LiBO2 and Na2CO3, since they are frequently used as fluxes in fusion procedures, and NH4Cl, ascorbic acid, and graphite. The effects of the chemical modification on the intensities of emission signals and the grinding time required for obtaining greater intensities emission signals were evaluated. The chemical modification procedure was implemented in order to promote the formation of new compounds with thermal properties different of the original materials. The synthesis of less refractory compounds would favor the process of atomization-excitation of the chemically modified materials in the direct analysis of slurries, and it would also facilitate the digestion of these materials. The effects of the chemical modification were also evaluated by using X-ray diffraction and thermogravimetric analysis. The direct analysis of chemically modified materials by ICP OES required the investigation of several calibration methods based on different approaches: use of aqueous reference solutions, calibration with slurries prepared using certified reference materials, and calibration using the generalized standard addition method. The calibration is the most critical aspect in the direct analysis of slurries by ICP OES, because is critically dependent on the particle sizes and of the thermal behavior of the several mineralogical phases of each material. On the other hand, microwave -assisted digestion was investigated in two alkaline media: KOH and NaOH. Applying a paired t-test it was shown that results were in agreement at 95% confidence level with those obtained by microwave-assisted acid digestion. The values of the detection limits and signal-to-background ratio obtained for the two microwave -assisted procedures were compared, and the alkaline digestion has shown adequate performance for the digestion of the chemically modified materials. / A proposta desta tese foi investigar procedimentos alternativos para análise química de materiais refratários e argilas por espectrometria de emissão óptica com plasma acoplado indutivamente (ICP OES) com configuração axial pela análise direta de suspensões e digestão assistida por radiação microondas empregando meio alcalino. A primeira etapa do trabalho foi avaliar a introdução de suspensões em ICP OES com configuração axial e os efeitos causados pela distribuição de tamanho de partículas sobre as intensidades dos sinais, sendo que o desempenho desse arranjo foi avaliado para suspensões de materiais refratários e argilas com diferentes tamanhos de partículas. A segunda etapa foi o desenvolvimento de um método de moagem das amostras sólidas juntamente com modificadores químicos. Dentre os modificadores químicos estudados encontram-se o LiBO2 e o Na2CO3, que são utilizados como fundentes em procedimentos de decomposição por fusão, NH4Cl, ácido ascórbico e grafite. Foram avaliados os efeitos da modificação química sobre as intensidades dos sinais de emissão dos analitos em suspensões dos materiais cerâmicos quimicamente modificados e o tempo de modificação necessário para obtenção de maiores valores de intensidades dos sinais de emissão. Esse procedimento de modificação química foi implementado a fim de promover a formação de novos compostos com propriedades térmicas diferentes dos materiais originais, ou seja, compostos menos refratários. Isso favoreceria o processo de atomização-excitação dos materiais quimicamente modificados na análise direta de suspensões e também facilitaria a digestão desses materiais. Os efeitos da modificação química também foram avaliados por estudos de difração de raios-X e análise ermogravimétrica. Na análise direta de suspensões dos materiais quimicamente modificados foram avaliados diversos meios que pudessem viabilizar a calibração do ICP OES com soluções de referência preparadas em meio aquoso, calibração com materiais de referência certificados e calibração empregando o método generalizado das adições do analito. Cabe ressaltar que o aspecto mais crítico da análise direta de suspensões por ICP OES é o procedimento de calibração, que é criticamente dependente do tamanho de partículas nas suspensões e da refratariedade das várias fases mineralógicas de cada material. Nos procedimentos assistidos por radiação microondas em meio alcalino, foram avaliadas dois reagentes: KOH e NaOH. Aplicando-se o teste t com 95% de confiança conclui-se que os resultados são concordantes com aqueles obtidos por procedimentos de digestão ácida assistido por radiação microondas. Para comparar os dois meios foram avaliados os valores de limite de detecção e razões sinal analítico-sinal de fundo para os dois meios, sendo que o meio alcalino se mostrou adequado para a digestão das amostras quimicamente modificadas.

Nesse trabalho, foram caracterizadas 238 amostras de Ãgua produzida, oriundos de quatro campos de produÃÃo diferentes, todos provenientes de campos marÃtimos da bacia do CearÃ, denominados campo de produÃÃo A, campo de produÃÃo B, campo de produÃÃo C e campo de produÃÃo D. Foram determinados, os Ãnions (Acetato, Cloreto, Formiato, Sulfato) utilizando-se a cromatografia de Ãons; exceto, para o Ãnion Bicarbonato que foi determinado utilizando-se a titulaÃÃo potenciomÃtrica. E, os cÃtions (BÃrio, CÃlcio, EstrÃncio, Ferro Total, LÃtio, MagnÃsio, PotÃssio, SÃdio) utilizando-se a espectrometria de emissÃo Ãptica com plasma acoplado indutivamente. Para tratamento estatÃstico, utilizou-se como ferramenta, a PCA (anÃlise de componentes principais) e a HCA (anÃlise de agrupamento hierÃrquico). Na avaliaÃÃo da qualidade dos dados, utilizou-se o balanÃo iÃnico. Para visualizaÃÃo dos resultados, utilizou-se o grÃfico boxplot, onde se pode observar que o campo de produÃÃo A, seguido do campo de produÃÃo B, possuem tendÃncia à corrosÃo e à incrustaÃÃo, respectivamente. Como tambÃm, o campo de produÃÃo D que apresentou propensÃo à corrosÃo, mas em menor escala. Vale salientar a necessidade de uma caracterizaÃÃo individual das amostras, para conhecimento dos principais constituintes existentes. Pois, esses constituintes podem acarretar elevados custos na manutenÃÃo do processo produtivo da indÃstria petrolÃfera; devido, a corrosÃo do tipo pite, que promove a modificaÃÃo da aparÃncia e estrutura dos aÃos inoxidÃveis, muito utilizados na indÃstria petrolÃfera; e, as incrustaÃÃes, que tendem a se depositar nas paredes das tubulaÃÃes, que podem causar problemas como perda de pressÃo, diminuiÃÃo do escoamento da produÃÃo e aumento no consumo de energia. / In this study, we characterized 238 samples of water produced from four different production fields, all from offshore fields of the Cearà basin, called The field of production, production field B, C production and field production field D. were determined anions (acetate, chloride, formate, sulfate) using ion chromatography; except for the bicarbonate anion was determined using potentiometric titration. And, cations (Barium, Calcium, Strontium, total iron, lithium, magnesium, potassium, sodium) using the optical emission spectrometry with inductively coupled plasma. For statistical analysis, we used as a tool, the PCA (principal component analysis) and HCA (hierarchical cluster analysis). In evaluating the quality of the data, we used the ionic balance. To visualize the results, we used the box plot graph where one can observe that the production field, followed by the production field B, are prone to corrosion and fouling, respectively. As well, the D production field that showed propensity to corrosion, but on a smaller scale. It is worth stressing the need for individual characterization of the samples, to knowledge of the main existing constituents. For these constituents can incur high costs in maintaining the productive process of the oil industry; due to corrosion pitting type, which promotes change the look and structure of stainless steel, widely used in the oil industry; and incrustations which tend to deposit on the walls of pipes, which may cause problems such as pressure loss, decreased production flow and an increase in power consumption.

O Brasil é um dos grandes produtores mundiais de minério de ferro e exporta a maior parte da sua produção. No comércio internacional é importante assegurar a comparabilidade dos resultados analíticos obtidos em diferentes laboratórios. Uma variação de 0,1 % na média do teor de ferro pode aumentar ou diminuir em muito o valor de um grande carregamento de minério. Assim, os sistemas de garantia da qualidade dos laboratórios necessitam de materiais de referência. Este trabalho estudou a preparação de um lote de minério de ferro (pelotizado) como material de referência, certificando os teores de vários constituintes por meio de um programa interlaboratorial. Treze laboratórios participaram do programa e dezoito componentes do minério tiveram seus teores certificados: Fetotal (65,1%), SiO2 (2,76%), Al2O3 (0,46%), TiO2 (0,056%), P (0,026%), S (0,003%), MnO (0,094%), CaO (3,31%), MgO (0,043%), K2O (0,013%), Ba (0,004%), Zn (13 mg/kg), Cu (10 mg/kg), Co (12 mg/kg), Cr (56 mg/kg), Pb (15 mg/kg), Ni (14 mg/kg), V (48 mg/kg). / Brazil is one of the great worldwide iron ore producers and exports most of its production. In the international trade it is important to make sure the comparison of the analytical results among different laboratories. A variation of 0,1% in the average of the iron content can increase or decrease the value of a large ore shipment. Thus, the quality guarantee systems of the laboratories need certified reference materials. The aim of this work was the preparation an amount of iron ore (pellets) as reference material, being certified content of some constituents through an interlaboratory program. Thirteen laboratories participated of the program and eighteen components of the ore had its content certified: Fetotal (65,1%), SiO2 (2,76%), Al2O3 (0,46%), TiO2 (0,056%), P (0,026%), S (0,003%), MnO (0,094%), CaO (3,31%), MgO (0,043%), K2O (0,013%), Ba (0,004%), Zn (13 mg/kg), Cu (10 mg/kg), Co (12 mg/kg), Cr (56 mg/kg), Pb (15 mg/kg), Ni (14 mg/kg), V (48 mg/kg).

This master thesis deals with analysis of Czech garlic varieties in comparison with two varieties from abroad. Alliin and carbohydrates were determined by high performance liquid chromatography with diode-array detector or evaporative light scattering detector. Crude proteins were calculated from total content of nitrogen that was determinated by Kjeldahl method. Elementary analysis was performed by inductively coupled plasma optical emission spectrometry. In theoretical part of this thesis is describes botanical characterization and cultivation of garlic, chemical composition of garlic, especially groups of substances which were analysed in this thesis. Principle of used methods is described too. The experimental part of this work deals with sample and calibration solution preparation and process of analysis. Obtained results from analysed substances are summarized in the tables, discussed and compared with results of analysis of other authors. Between Czech and Spanish/Chinese garlic are slight differences. Garlics contain 24,66 g/kg dry weight of alliin. Content of crude proteins in Czech garlic is comparable to Chinese garlic but the Spanish garlic has just half of amount crude proteins. Elementary analysis also includes significant differences. Czech varieties contain higher amount of phosphorus, iron and zinc. On the contrary, content of potassium in foreign garlic is higher than in Czech Republic and the analysed amount is 15 g/kg dry weight.

This diploma thesis is focused on the analysis of egg yolks and egg whites from chickens raised with different breeding methods in the Czech Republic using three analytical methods. The Kjeldahl method was used to determine the proteins, the Soxhlet method was used to determine the lipids and ICP-OES was used for elemental analysis. The theoretical part describes the history of chicken breeding, marking and distribution of eggs and composition of eggs based on various aspects. The main point was the separation of egg yolk and egg white and the subsequent description on the chemical and physiological level. Principle of used methods is also described. The experimental part deals with the preparation of samples, calibration samples and process analysis. All the results of analysed substances are summarized, statistically evaluated and compared with the other literature. For this analysis were used eleven different types of eggs from the Czech Republic from six different categories.

This disertation deals with geographical authentification of different types of spices and spice preparations. Investigated spice species were garlic (Allium sativum), ground pepper (Capsicum anuum), and dried carrot (Daucus carota). Theoretical part of the disertation describes main qualitative parameters of the examined species and production technology, means of food adulteration and statistic methods used in chemometrics. The aim of this dissertation was to verify the hypothesis whether it is possible to use targeted analytical techniques commonly used in quality control of spices and condiments, and statistical processing of measured data to distinguish samples of spices and condiments of different geographical origin. The use of non-targeted analysis was also investigated. Samples of garlic and ground pepper were used for targeted analysis. The examined parameters were dry matter and moisture of the sample, ash content, total phenolic content according to Folin-Ciocaulteu, carbohydrate content, alliin concentration, total nitrogen content, total color pigment (ASTA), pH of aqueous extract, total fat content, and concentration of selected elements (Ca, Cu, Fe, K, Mn, Mg, Na, P, Zn). The instrumental techniques used were molecular absorption spectrometry, inductively coupled plasma optical emission spectrometry and high performance liquid chromatography. The obtained data were statistically processed by analysis of variance (ANOVA) and principal component analysis (PCA). Using statistical analysis significant differences between samples that came from more distant areas were found. However, samples from closer areas could not be distinguished. The researched hypothesis could not be unequivocally confirmed or refuted. Metabolic fingerprint of carrot samples was determined using non-targeted analysis. Metabolic analysis was performed using the tandem LC-TOF-MS technique. The data were processed by recursive peak extraction (BRE) and subsequently uvaluated with PCA. The samples were divided into clusters according to their origin. Targeted and non-targeted techniques have great potential in verifying the geographical authenticity of different types of spices. However, the main condition is consistent and sufficient sampling, guaranteed information on the origin of the sample and obtaining a sufficient amount of input data for statistical analysis.

This doctoral thesis studies the properties and behaviour of phase-separated hydrogels. These can be prepared by interaction of polyelectrolytes with oppositely charged surfactants. Negatively charged polysaccharide hyaluronan and cationic surfactant carbethopendecinium bromide (Septonex), whose properties, behaviour and utilization are described in the first two chapters of theoretical part, were selected for this role. Hyaluronan is naturally-occuring in living organisms and is known for his specific targeting to the tumour cells. Septonex is used as antiseptic and disinfectant. Experimental part of this work is focused on examination of the structure and behaviour of these types of hydrogels especially from rheological point of view. The crucial part of this study was to establish mechanical properties and their dependence on environment. This led to design further studies. Structural analysis was held using the methods of ATR-FTIR, ionic chromatography and ICP-OES helping to measure the inner content of entry materials in the gels and supernatants respectively. The last chapter deals with antimicrobial activity. The results of this study indicate a potential usage of these substances in the field of medical applications.

The theoretical part of the thesis deals with the chemical composition of cow’s milk, with the description of chosen methods of sample pretreatment and with the description of the used technique ICP-OES. The practical part is aimed at individual preparations of samples and at analysis of chosen chemical elements (Ca, Na, K and Mg). Milk is a really complicated polydisperse system, that’s the reason why the preparation of samples with milk is very important step before the measurement itself. In addition to accuracy choosing the sample adjustment method, other factors such as time, work intensity, or cost need to be considered when. In the thesis a comparison of four selected methods of sample preparation was made: direct analyse of milk, dilution with addition of Triton X-100, wet microwave ashing and destruction of matrix with TMAH (tetramethylammonium hydroxide). Selected elements were analysed with the help of ICP-OES. This diploma thesis builds on the bachelor thesis, which deals with the same problem. Final concentrations were compared with certified values of skimmed powdered milk. Data showed that the most accurate are methods of preparation of wet microwave ashing and destruction of matrix with TMAH. By using these methods, the effect of the dairy matrix that caused problems in the analysis, was largely eliminated. The diluted samples with and without Triton X-100 showed a bigger anomaly of measuring than the mineralization of wet ashing which came to the loss of analyte because of fat elements contained in milk.