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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.
121

Petrologia e geoqu?mica do magmatismo ediacarano Serra do Caramuru, Rio Grande do Norte, NE do Brasil

Mac?do Filho, Antomat Avelino de 19 February 2016 (has links)
Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-08-16T20:54:14Z No. of bitstreams: 1 AntomatAvelinoDeMacedoFilho_DISSERT.pdf: 31646406 bytes, checksum: f6ba113eebabf49dff56fd9add20f343 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-08-19T00:32:03Z (GMT) No. of bitstreams: 1 AntomatAvelinoDeMacedoFilho_DISSERT.pdf: 31646406 bytes, checksum: f6ba113eebabf49dff56fd9add20f343 (MD5) / Made available in DSpace on 2016-08-19T00:32:03Z (GMT). No. of bitstreams: 1 AntomatAvelinoDeMacedoFilho_DISSERT.pdf: 31646406 bytes, checksum: f6ba113eebabf49dff56fd9add20f343 (MD5) Previous issue date: 2016-02-19 / Os stocks Serra do Caramuru e Tapuio, localizados no extremo NE do Dom?nio Rio Piranhas-Serid? (RN), s?o representantes do magmatismo ediacarano a cambriano, uma fei??o magm?tica marcante da orog?nese Brasiliana / Panafricana na Prov?ncia Borborema. Estes corpos s?o an?logos litol?gicos, intrusivos no embasamento gn?issico paleoproterozoico, estando separados por uma t?nue faixa de ortognaisses milon?ticos. As rela??es de campo mostram uma estratigrafia magm?tica iniciada pela f?cies dior?tica que coexiste com as f?cies gran?tica porfir?tica e gran?tica equigranular I e, em menor frequ?ncia, com a f?cies gran?tica equigranular II. Estas rochas s?o cortadas por diques e sheets gran?ticos tardios NE-SW a NNE-SSW. A f?cies dior?tica (dioritos, quartzo dioritos, quartzo monzodioritos, tonalitos e granodioritos) ? leucocr?tica a melanocr?tica, rica em biotita e anfib?lio. As f?cies gran?ticas s?o hololeucocr?ticas a leucocr?ticas, com biotita ? anfib?lio. Dados petrogr?ficos e geoqu?micos (rocha total) provenientes em maior propor??o do plut?o Serra do Caramuru, sugerem o fracionamento de zirc?o, apatita, clinopirox?nio (em dioritos), opacos, titanita, biotita, hornblenda, allanita, plagiocl?sio, microcl?nio e granada (em diques). O comportamento dos elementos tra?os Zr, La e Yb indicam que dioritos n?o constituem o magma parental dos granitos. Por outro lado, as f?cies gran?ticas s?o cogen?ticas entre si, apresentando trends de diferencia??o e espectros de elementos terras raras (ETR) an?logos [12.3?(La/Yb)N?190.8; Eu/Eu*=0.37-0.68]. Rela??es de campo e padr?o de ETR [6.96?(La/Yb)N?277.8; Eu/Eu*=0.18-0.58] demonstram que os diques e sheets gran?ticos n?o s?o cogeneticamente relacionados ao magmatismo Serra do Caramuru. A f?cies dior?tica ? metaluminosa (A/CNK = 0.88-0.74), shoshon?tica, ao passo que granitos s?o metaluminosos a peraluminosos (A/CNK = 1.08-0.93), c?lcio-alcalinos de alto pot?ssio. Diques e sheets s?o estritamente peraluminosos (A/CNK = 1.01-1.04). Diagramas bilogar?tmicos relacionando elementos compat?veis e incompat?veis e microtexturas indicam a cristaliza??o fracionada como o mecanismo dominante na evolu??o magm?tica das diversas f?cies. Os stocks Serra do Caramuru e Tapuio mostram trama magm?tica bem preservada, aus?ncia de minerais metam?rficos e s?o estruturalmente isotr?picos, com rela??es de contato discordantes da trama d?ctil do embasamento gn?issico. Estas observa??es conduzem a um est?gio de relativa estabilidade tect?nica, compat?veis com o per?odo de relaxamento orogen?tico da cadeia Brasiliana / Panafricana. Os diagramas qu?micos discriminantes envolvendo ?xidos e elementos tra?os indicam um ambiente tardio ? p?s-colisional. Neste contexto, o mecanismo de coloca??o que melhor explica o alojamento dos stocks seria a abertura de espa?o em fraturas de Ridel tipo T, com vetor de estiramento orientado ENE-WSW. A idade U-Pb de 553 ? 10 Ma permite correlacionar o magmatismo Serra do Caramuru aos grupo de granitoides tardios a p?s-colisionais, c?lcio-alcalinos de alto pot?ssio equigranulares, do extremo NE do Dom?nio Rio Piranhas-Serid?. / The Serra do Caramuru and Tapuio stocks, located in the extreme NE of Rio Piranhas-Serid? Domain (RN), are representative of the Ediacaran-Cambrian magmatism, an important magmatic feature of the Brasilian / Panafrican orogeny of the Borborema Province. These bodies are lithologically similar, intrusive in paleoproterozoic gneiss embasement, being separated by a thin belt of mylonitic orthogneiss. The field relations show a magmatic stratigraphy initiated by dioritic facies that coexists with the porphyritic granitic and equigranular granitic I facies, and less frequently with equigranular granitic II facies. These rocks are crosscut by late granitic dykes and sheets with NE-SW / NNE-SSW orientation. The dioritic facies (diorite, quartz diorite, quartz monzodiorites, tonalite and granodiorite) is leucocratic to melanocratic, rich in biotite and hornblende. The granitic facies are hololeucocratic to leucocratic, and have biotite ? hornblende. Petrographic and geochemical (whole rock) data, especially from Serra do Caramuru pluton, suggest fractionation of zircon, apatite, clinopyroxene (in diorites), opaque minerals, titanite, biotite, hornblende, allanite, plagioclase, microcline and garnet (in dykes). The behavior of trace elements such as Zr, La and Yb indicates that the dioritic magma does not constitute the parental magma for the granitic facies. On the other hand, the granitic facies seems to be cogenetic to each other, displaying differentiation trends and very similar rare earth elements (REE) spectra [12.3?(La/Yb)N?190.8; Eu/Eu*=0.30-0.68]. Field relationships and REE patterns [6.96?(La/Yb)N?277.8; Eu/Eu*=0.18-0.58] demonstrate that the granitic dykes and sheets are not cogenetically related to the Serra do Caramuru magmatism. The dioritic facies is metaluminous (A/CNK = 0.88-0.74) and shoshonitic, whereas the granitic ones are metaluminous to peraluminous (A/CNK = 1.08-0.93) and high potassium calc-alkaline. Dykes and sheets are strictly peraluminous (A/CNK = 1.01-1.04). Binary diagrams relating compatible and incompatible trace elements and microtextures indicate the fractional crystallization as the dominant mechanism of magmatic evolution of the various facies. The Serra do Caramuru and Tapuio stocks have well preserved magmatic fabric, do not show metamorphic minerals and are structurally isotropic, showing crosscutting contact with the ductile fabric of the basement. These observations lead to interpretate a stage of relative tectonic stability, consistent with the orogenic relaxation period of the Brasiliano / Pan-African orogeny. Chemical plots involving oxides and trace elements indicate late to post-collisional emplacement. In this context, the assumed better mechanism to describe the stocks emplacement within an extensional T Riedel joint, with ENE-WSW extensional vector. The U-Pb zircon age of 553 ? 10 Ma allows correlating the Serra do Caramuru magmatism to the group of post-collisional bodies, equigranular high potassium calc-alkaline granites of the NE of Rio Piranhas-Serid? Domain.
122

Petrografia, litoqu?mica, qu?mica mineral e termobarometria de rochas c?lcioalcalinas de alto K de textura porfir?tica, ediacaranas, no extremo NE da Prov?ncia Borborema (NE do Brasil)

Campos, Benedita Cleide de Souza 26 February 2016 (has links)
Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-08-26T23:58:51Z No. of bitstreams: 1 BeneditaCleideDeSouzaCampos_DISSERT.pdf: 4403566 bytes, checksum: c3c751a75b003cb890a6499c81c7642f (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-08-31T22:03:44Z (GMT) No. of bitstreams: 1 BeneditaCleideDeSouzaCampos_DISSERT.pdf: 4403566 bytes, checksum: c3c751a75b003cb890a6499c81c7642f (MD5) / Made available in DSpace on 2016-08-31T22:03:44Z (GMT). No. of bitstreams: 1 BeneditaCleideDeSouzaCampos_DISSERT.pdf: 4403566 bytes, checksum: c3c751a75b003cb890a6499c81c7642f (MD5) Previous issue date: 2016-02-26 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / A qu?mica mineral de granitos, juntamente com revis?o de dados qu?micos de rocha total e petrografia foram utilizados para determinar as condi??es de cristaliza??o e as implica??es na g?nese de granitos C?lcio-alcalinos de alto K Porfir?ticos. Seis corpos gran?ticos foram analisados: Monte das Gameleiras, Barcelona, Acari, Cara?bas, Tour?o e Catol? do Rocha, localizados nos dom?nios Rio Piranhas-Serid? e S?o Jos? de Campestre, NE do Brasil. Os pl?tons s?o representados por monzogranitos, texturalmente possuem f?cies porfir?tica compreendendo fenocristais de K-feldspato com tamanhos entre 5 a 15 cm. K-feldspato, plagiocl?sio e quartzo constituem a parag?nese f?lsica e dominante; enquanto biotita e anfib?lio representam os minerais m?ficos principais; titanita, minerais opacos, allanita, ep?doto, apatita e zirc?o s?o os principais acess?rios. Em rela??o ao ?ndice de Shand o granito Monte das Gameleiras mostra-se mais metaluminoso, enquanto os outros seguem a transi??o metaluminoso a peraluminoso. Em diagramas discriminantes qu?micos estes se apresentam com car?ter transicional (subalcalino). As an?lises de petrografia e qu?mica n?o exp?e as diferen?as dos granitos, por?m os resultados de qu?mica mineral revelam as diferen?as dos mesmos e podem ser divididos em dois grupos: a leste (Monte das Gameleiras, Barcelona e Acari) e a oeste (Cara?bas, Tour?o e Catol? do Rocha). As raz?es Fe/(Fe+Mg) da biotita mostra um aumentam do grupo leste para oeste com valores de 0,48 a 0,64 e 0,66 a 0,92 respectivamente. As raz?es Mg/(Mg+Fe2) do anfib?lio diminui nesse sentido com valores de 0,40 a 0,57 e 0,06 a 0,31. As condi??es de cristaliza??es para os granitos a leste (Monte das Gameleiras, Barcelona e Acari) mostram press?o entre 4.2 kbar a 5.8 kbar, com profundidades que variam de 15,9 km a 20,5 km a uma temperatura entre 710 ?C a 734?C e a oeste (Cara?bas, Tour?o e Catol? do Rocha) com press?es de 5,4 kbar a 7,1 kbar e profundidades que variam de 20 km a 23 km a uma temperatura entre 729 ?C - 753 ?C. Ambas as ?reas, tanto leste como oeste foram gerados a partir de magmas oxidados. As profundidades das intrus?es gran?ticas podem estar relacionadas aos deslocamentos de falhas e ao alto conte?do de ?gua e vol?teis que permitem que o magma de alguns plutons atinja n?veis mais rasos em rela??o aos outros. Os resultados mostram um aumento sistem?tico de temperatura e press?o de cristaliza??o dos pl?tons de leste para oeste sugerindo um espessamento crustal nessa dire??o nos dois dom?nios geol?gicos pesquisados. / The mineral chemistry from granites, chemical of whole rock and review of petrography were used to determine the crystallization conditions and the implications in the genesis of high-K calc-akaline granites that are porphyritics, localizated in the Rio Piranhas-Serid? (RPSD) and S?o Jos? de Campestre Domains (SJCD). Six granitic bodies were analyzed and that for the intrusive granites within the SJCD were named East granites: Monte das Gameleiras, Barcelona. The Acari granite intrudes the area RPSD, however, was called as granite east due to the characteristics of mineral chemistry is similar to east granites. Granites Cara?bas, Tour?o and Catol? do Rocha are intrusive in the RPSD and called west granites. The six bodies are located in the northeast of the Borborema Province, NE Brazil. The plutons are represented by monzogranites wich have porphyritic facies with phenocrysts of K-feldspar with sizes between 5 and 15 cm. The K-feldspar, plagioclase and quartz are the dominant paragenesis; while the biotite and amphibole are the main mafic minerals; and titanite, opaque minerals, allanite, epidote, apatite and zircon are the accessories minerals. The Monte das Gameleiras granite shows metaluminous aluminium saturation index, whereas the others plutons metaluminous to peraluminous. In geochemical diagrams, the granites present with transitional character (subalcalino). The petrographic and geochemical analysis didn't show the differences between the plutons, but according to the mineral chemistry they can be divided into two groups: Monte das Gameleiras, Barcelona and Acari (east) and Cara?bas, Tour?o e Catol? do Rocha (west). The Fe/(Fe + Mg) ratio of biotite shows an increase from east to west group with values from 0.45 to 0.64 and 0.66 to 0.92 respectively, and the Mg / (Mg + Fe2) of amphibole decreases with values from 0.40 to 0.57 and from 0.07 to 0.31. The crystallization parameters of east granites, The crystallization conditions for granites east (Monte das Gameleiras, Barcelona and Acari) show pressure between 3.8 kbar to 5.5 kbar, with depths ranging from 14 km to 21 km at a temperature between 701 ? C to 742?C and west (Cara?bas, Tour?o and Catol? Rock) with pressures to 4.8 kbar to 6.2 kbar and depths ranging from 18 km to 23 km at a temperature between 723 ? C - 776 ? C. Both areas, east and west were generated from magmas oxidized with ?FQM values (-1 a +2.0). The depths of granite intrusion failures may be related to offsets and high water content and volatile that allow the magma some plutons reaches shallower levels in relation to the other. The results show a systematic increase in temperature and crystallization pressure east of plutons west suggesting crustal thickening in that direction. The results show a systematic increase in temperature and crystallization pressure east to west plutons, suggesting crustal thickening in that direction in the two domains studied.
123

A nova geografia econ??mica: tr??s ensaios para o Brasil

Aguilar, Carla Cristina January 2007 (has links)
Submitted by Gustavo Gomes (gustavolascasas@gmail.com) on 2013-09-17T12:16:48Z No. of bitstreams: 2 A Nova Geografia Econ??mica tr??s ensaios para o Brasil.pdf: 1310322 bytes, checksum: 3f258950dd48382377323781b037cf47 (MD5) license_rdf: 23599 bytes, checksum: 9e2b7f6edbd693264102b96ece20428a (MD5) / Approved for entry into archive by Roger Guedes (roger.guedes@fjp.mg.gov.br) on 2013-09-17T13:48:42Z (GMT) No. of bitstreams: 2 A Nova Geografia Econ??mica tr??s ensaios para o Brasil.pdf: 1310322 bytes, checksum: 3f258950dd48382377323781b037cf47 (MD5) license_rdf: 23599 bytes, checksum: 9e2b7f6edbd693264102b96ece20428a (MD5) / Made available in DSpace on 2013-09-17T13:48:42Z (GMT). No. of bitstreams: 2 A Nova Geografia Econ??mica tr??s ensaios para o Brasil.pdf: 1310322 bytes, checksum: 3f258950dd48382377323781b037cf47 (MD5) license_rdf: 23599 bytes, checksum: 9e2b7f6edbd693264102b96ece20428a (MD5) Previous issue date: 2007 / Funda????o Jo??o Pinheiro / Esta tese tem como proposta analisar a desigualdade da distribui????o das atividades econ??micas e da renda per capita no Brasil, utilizando dados censit??rios para as microrregi??es do Nordeste, Sudeste e Centro-Oeste. Para isso, s??o apresentados tr??s artigos. No primeiro artigo, Acessibilidade e desigualdade regional no Brasil: uma proposta metodol??gica, prop??e-se um indicador de acessibilidade que ?? uma medida de mercado potencial, mas que considera as diferen??as de infra-estrutura existentes no Brasil. O segundo, Aglomera????es: quais seus fatores explicativos?, atrav??s de uma metodologia de an??lise de vari??ncia, procura responder quais os fatores explicativos das aglomera????es. Os resultados mostram que os principais fatores s??o os aglomerativos, corroborando com os argumentos da Nova Geografia Econ??mica. Diante disso, buscaram-se ind??cios de que o custo de transporte esteja no n??vel intermedi??rio, o que foi verificado. O terceiro artigo, Mercado potencial e crescimento econ??mico: evid??ncias para as microrregi??es do Sudeste, Nordeste e Centro-Oeste brasileiro, analisa se existem evid??ncias de que o acesso aos mercados influencia o diferencial de renda per capita existente entre as microrregi??es e se h?? heterogeneidade dos par??metros. Os resultados apontam para uma influ??ncia do acesso aos mercados sobre o diferencial de renda per capita. Essa influ??ncia ?? diferenciada entre as microrregi??es presentes no Sudeste e no Nordeste e Centro-Oeste. No Sudeste, h?? uma rela????o positiva, ou seja, quanto maior o acesso aos mercados maior o crescimento da renda per capita, enquanto para as microrregi??es do Nordeste e Centro-Oeste o resultado ?? inverso. / This thesis has three contributions: a) in the first paper, we develop a transportation cost index based on the market potential concept. b) In the second paper, we test if first or second nature causes determine agglomerations in our sample, which is composed by micro-regions of the Northeast, Southeast and Centre-West macro-regions in Brazil, in the period 1970-2000. We observe that second order causes directly or indirectly are the main determinants of agglomeration. We also collect evidence that transportation cost are at intermediate levels in these regions. c) In the third paper, we investigate if access to markets determines the (transitional) growth rate of per capita income. It does, but in a differentiated manner accordingly mainly to the macro-region from which the micro-region belongs. / Economia e Finan??as
124

Estudo qu?mico e de atividade biol?gica de Plectranthus neochilus Schltr. (Lamiaceae)

Viana, Abra?o Jos? Silva 16 September 2011 (has links)
Submitted by Rodrigo Martins Cruz (rodrigo.cruz@ufvjm.edu.br) on 2015-02-19T13:03:27Z No. of bitstreams: 5 abraao.pdf: 3789153 bytes, checksum: 0d883e26dd234b7e0859f99b195f74c4 (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) / Approved for entry into archive by Rodrigo Martins Cruz (rodrigo.cruz@ufvjm.edu.br) on 2015-02-19T13:44:19Z (GMT) No. of bitstreams: 5 abraao.pdf: 3789153 bytes, checksum: 0d883e26dd234b7e0859f99b195f74c4 (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) / Made available in DSpace on 2015-02-19T13:44:19Z (GMT). No. of bitstreams: 5 abraao.pdf: 3789153 bytes, checksum: 0d883e26dd234b7e0859f99b195f74c4 (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) Previous issue date: 2013-02-19 / O trabalho apresentado nesta disserta??o descreve o estudo fitoqu?mico e de atividade biol?gica das folhas e caules e flores de Plectranthus neochilus Schltr., esp?cie pertencente ? fam?lia Lamiaceae. A planta ? uma erva arom?tica conhecida popularmente no Brasil como ?boldo? ou ?boldo-gamb??, e assim como as esp?cies P. barbatus Andrews (?boldo-brasileiro") e P. ornatus Codd. ("boldinho"), tem o ch? de suas folhas utilizadas na medicina tradicional no tratamento de insufici?ncia hep?tica e dispepsia, em substitui??o a Peumus boldus Molina (?boldo-do-chile?). O estudo fitoqu?mico do extrato hex?nico das folhas e caules de P. neochilus forneceu dois triterpenos: ?-amirina (PN1) e friedelina (PN2). PN1 foi isolada como um ?ster de ?cido graxo ligado na posi??o C-3. Deste extrato foi obtida tamb?m a mistura dos ester?ides sitosterol e estigmasterol (PN3). O estudo fitoqu?mico conduzido com o extrato em acetato de etila das folhas e caules forneceu a flavona metoxilada nas posi??es C-6 e C-7, a cirsimartina (PN4). Todos os compostos obtidos foram descritos pela primeira vez na esp?cie. A elucida??o estrutural dos compostos isolados, baseou-se na an?lise espectrosc?pica de RMN 1D, CLAE, ESI e por compara??o com dados encontrados na literatura. O extrato metan?lico das folhas e caules de P. neochilus mostrou significativa atividade antioxidante quando avaliado pelo m?todo de DPPH, seguido pelo extrato em acetato de etila e hex?nico. Foi avaliado tamb?m o extrato metan?lico das flores da esp?cie, que apresentou atividade inferior aquele observado para o extrato metan?lico das folhas e caule, sendo estas atividades confirmadas pelo conte?do fen?lico dos extratos. A atividade anticolinester?sica dos extratos das folhas e caules e das flores de P. neochilus foi avaliada, sendo observada a inibi??o da enzima acetilcolinesterase para todos os extratos pesquisados. / Disserta??o (Mestrado) ? Programa de P?s-Gradua??o em Qu?mica, Universidade Federal dos Vales do Jequitinhonha e Mucuri, 2011. / ABSTRACT The present work describes the phytochemical and pharmacological investigation on extracts of the leaves and stems and flowers of the species Plectranthus neochilus Schltr. belonged to the family Lamiaceae. The plant is aromatic herb popularly known in Brazil as ?boldo? or ?boldo-gamb??, and as the species P. barbatus Andrews (?boldo-brasileiro") e P. ornatus Codd. ("boldinho"), according to ethnopharmacological survey, is often used in the treatment of hepatic insufficiency and dyspepsia, replacing the Peumus boldus Molina (?boldo-do-chile?). The phytochemical investigation of the hexanic extract of the P. neochilus leaves and stems yielded two triterpenes: ?-amyrin (PN1) e friedelin (PN2). The compound ?-amirin was isolated as a fatty acid ester in position C-3. In this extract was also obtained the mixture of the steroids sitosterol and stigmasterol (PN3). The phytochemical study conducted with the ethyl acetate extract of the leaves and stems gave the methoxy flavone at positions C-6 and C-7, the cirsimartin (PN4). All compounds obtained were first described in the species. Structural elucidation of isolated compounds was based on spectroscopic analysis of 1D NMR, HPLC, ESY and by comparison with data found in literature. The methanol extract of leaves and stems of P. neochilus showed significant antioxidant activity when evaluated by the DPPH method, followed by the extract in ethyl acetate and hexane. We also evaluate the methanol extract of flowers of the species that showed activity lower than that observed for the methanolic extract from leaves and stems, and these activities confirmed for the content of phenolic extracts. The anticholinesterase activity of extracts of leaves and stems and flowers of P. neochilus was evaluated and found to inhibit the enzyme acetylcholinesterase to all extracts studied.
125

Determina??o de sildenafila (Viagra?) e carbamazepina em formula??es farmac?uticas por amperometria de m?ltiplos pulsos em sistema FIA / Determination of sildenafil (Viagra?) and carbamazepine in pharmaceutical formulations by multiple pulses amperometry in FIA system

Lopes J?nior, Ant?nio Carlos Vieira 27 July 2012 (has links)
Submitted by Rodrigo Martins Cruz (rodrigo.cruz@ufvjm.edu.br) on 2015-02-19T13:03:28Z No. of bitstreams: 5 carlos.pdf: 2538374 bytes, checksum: bc72a52cc529db58b3cf890bd9a41042 (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) / Approved for entry into archive by Rodrigo Martins Cruz (rodrigo.cruz@ufvjm.edu.br) on 2015-02-20T09:21:34Z (GMT) No. of bitstreams: 5 license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) carlos.pdf: 2538374 bytes, checksum: bc72a52cc529db58b3cf890bd9a41042 (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) / Made available in DSpace on 2015-02-20T09:21:34Z (GMT). No. of bitstreams: 5 license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) carlos.pdf: 2538374 bytes, checksum: bc72a52cc529db58b3cf890bd9a41042 (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) Previous issue date: 2013-02-21 / O presente trabalho apresenta m?todos simples, r?pidos e de baixo custo para determina??o de citrato de sildenafila (CS) e carbamazepina (CBZ) em formula??es farmac?uticas atrav?s da detec??o amperom?trica de m?ltiplos pulsos (MPA) em sistema de an?lise por inje??o em fluxo (FIA) utilizando como eletrodo de trabalho o diamante dopado com boro (DDB). O m?todo para determina??o de CS consiste na aplica??o de tr?s pulsos de potencial em sequ?ncia. Os pulsos de potencial de 1,6 V e 1,9 V s?o utilizados para detec??o eletroqu?mica do f?rmaco e um terceiro pulso de potencial (1,0 V) para promover a limpeza e reativa??o da superf?cie do eletrodo de DDB. Os limites de detec??o (LD) obtido nas condi??es estabelecidas est?o na ordem de 10 nmol L-1 para ambos os potenciais de detec??o. O desvio padr?o relativo das respostas de 10 inje??es consecutivas de CS na concentra??o de 4,5x10-5 mol L-1 foi de 0,1 e 0,2% para os pulsos de potencial de detec??o de 1,9 V e 1,6 V, respectivamente. Os estudos de adi??o e recupera??o de CS padr?o foram realizados em todas as amostras farmac?uticas apresentando recupera??o, em todos os casos, pr?ximo de 100%. Os resultados de doseamento dos medicamentos realizados a partir do m?todo proposto foram validados por metodologia cromatogr?fica. Para a CBZ foram propostas duas vertentes anal?ticas, uma voltada para determina??o do ativo em amostras farmac?uticas e outra para detec??o do f?rmaco em fluidos biol?gicos. Alguns par?metros foram semelhantes em ambos os procedimentos, s?o eles: eletr?lito suporte (?cido sulf?rico 0,2 mol L-1), vaz?o (3,0 mL min-1), volume de amostragem (150 ?L), potencial de limpeza (-1,4 V) e tempo de aplica??o deste potencial (600 ms). Al?m destes par?metros, para an?lise do f?rmaco em produto farmac?utico, foram utilizados para detec??o os pulsos de potenciais 1,6 e -1,2V, sendo aplicados por 150 e 30 ms, respectivamente. Nestas condi??es, foram obtidas as seguintes faixas lineares de trabalho: 0,6 a 40,0 ?mol L-1 para o pulso de potencial de 1,6 V e 0,4 a 20,0 ?mol L-1 para o pulso de potencial de -1,2 V. Para determina??o de CBZ em fluido biol?gico adotou-se como sistema de detec??o o pulso de potencial de 1,6 V aplicado por 800 ms (gerador) e o pulso de potencial de -1,2 V aplicado por 30 ms (detector). Para este pulso de potencial foi obtida faixa linear de trabalho de 0,02 a 1,0 ?mol L-1 e LD de 1,78 nmol L-1. Os estudos de adi??o e recupera??o de CBZ padr?o em amostras farmac?uticas e urina apresentaram resultados pr?ximos de 100%. Os resultados do ensaio de doseamento de medicamentos, realizados pelo m?todo proposto, foram validados por meio de metodologia oficial. Este trabalho apresenta, pela primeira vez, m?todos para determina??o de CS e CBZ em formula??es farmac?uticas atrav?s da detec??o MPA em sistema FIA. A associa??o desta t?cnica ao eletrodo de trabalho de DDB permitiu o desenvolvimento de m?todos de elevada sensibilidade, seletividade, rapidez e reprodutibilidade, demonstrando not?vel potencialidade para aplica??o no controle de qualidade de rotina de CS e CBZ em laborat?rios farmac?uticos e farm?cias de manipula??o. / Disserta??o (Mestrado) ? Programa de P?s-Gradua??o em Qu?mica, Universidade Federal dos Vales do Jequitinhonha e Mucuri, 2012. / ABSTRACT The present work presents simple, fast and low-cost methods for determination of sildenafil citrate (CS) and carbamazepine (CBZ) in pharmaceutical formulations using flow injection analysis (FIA) with multiple pulse amperometric (MPA) detection on the boron-doped diamond (DDB) working electrode. The method for the CS determination consists of the application of three sequential potential pulses as function of the time. SC is detected at 1.6 V and 1.9 V by two different irreversible oxidation processes. The third potential pulse (1.0 V) is applied for the regeneration (cleaning) of the electrode (boron-doped diamond) surface. The limit of detection (LD) in an order of 10 nmol L-1 was reached with a standard deviation of less than 0.2 % (n = 10) for 4.5 x 10-5 mol L-1 CS. The analytical frequency was calculated in 86 injections per hour. The addition-recovery studies in all the samples were around 100% and the results were validated by chromatographic methods. For the CBZ determination, two analytic conditions were proposed, one used for determination of a drug in pharmaceutical samples and other for detection the active ingredient in biological fluids. Some parameters were similar in both procedures, they are: supporting electrolyte (sulfuric acid 0.2 mol L-1), flow (3.0 ml min-1), sampling volume (150 ?L), regeneration potential pulse (-1.4 V) and time of application of this potential (600 ms). In addition to these parameters, for analysis of pharmaceutical drug, were used to detect it the potential pulses 1.6 V and -1.2 V, being applied for 150 and 30 ms, respectively. These conditions provided linear range of 0.6 to 40.0 ?mol L -1 for potential pulse 1.6 V and 0.4 to 20.0 ?mol L-1 for potential pulse -1.2 V. For the CBZ determination in biological fluid adopted as detection system the potential pulse of 1.6 V applied for 800 ms (generator) and potential pulse of -1.2 V applied for 30 ms (detector). For this potential pulse the linear range was of 0.02 to 1.0 ?mol L-1 and the LD was 1.78 nmol L-1. The addition-recovery studies in all the samples were around 100 % and the results were validated by official method. This work presents for the first time methods of SC and CBZ determination in pharmaceutical formulations utilizing MPA detection coupled to an FIA system. This technique, associated with a BDD working electrode, provided a sensitive, selective, fast and highly reproducible methods. Thus, the proposed methods may be an extremely attractive alternative for routine large and small-scale CS and CBZ analysis.
126

Desenvolvimento de um imunosensor pela t?cnica de resson?ncia de pl?smons de superf?cie para detec??o em tempo real de anticorpos anti - leishmania infantum / Development of an Immunosensor by the Surface Plasmon Resonance technique for real-time detection of anti-Leishmania infantum antibodies

Souto, D?nio Emanuel Pires 21 February 2012 (has links)
Submitted by Rodrigo Martins Cruz (rodrigo.cruz@ufvjm.edu.br) on 2015-02-19T13:03:29Z No. of bitstreams: 5 denio.pdf: 1745055 bytes, checksum: 531bb76e60dd34c17e7c27620ce5b5c0 (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) / Approved for entry into archive by Rodrigo Martins Cruz (rodrigo.cruz@ufvjm.edu.br) on 2015-02-20T10:55:25Z (GMT) No. of bitstreams: 5 denio.pdf: 1745055 bytes, checksum: 531bb76e60dd34c17e7c27620ce5b5c0 (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) / Made available in DSpace on 2015-02-20T10:55:25Z (GMT). No. of bitstreams: 5 denio.pdf: 1745055 bytes, checksum: 531bb76e60dd34c17e7c27620ce5b5c0 (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) Previous issue date: 2013-02-21 / Funda??o de Amparo ? Pesquisa do estado de Minas Gerais (FAPEMIG) / Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico (CNPq) / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (Capes) / Neste trabalho, foi realizado o desenvolvimento de um imunosensor para detec??o de anticorpos anti-Leishmania infantum. O princ?pio de transdu??o foi a Resson?ncia de Pl?smons de Superf?cie (SPR) e o sensor foi produzido atrav?s da imobiliza??o covalente de ant?genos sol?veis de Leishmania infantum sobre Monocamada Auto-Organizada (SAM) do ?cido 11-Mercaptoundecan?ico (11-MUA) ativado pela mistura contendo 100,0 mmol.L-1 de 1-etil-3-(3-dimetilaminopropil) carbodiimida (EDC) e 150 mmol.L-1 de N-hidroxisuccinimida (NHS). Atrav?s das t?cnicas de Voltametria C?clica e Redu??o Dessortiva por Voltametria de Pulso Diferencial o processo de forma??o da SAM foi otimizado. Sob condi??es otimizadas, 1,0 mmol.L-1 da solu??o etan?lica de 11-MUA e 24 horas foram suficientes para a forma??o de uma SAM est?vel sobre a superf?cie de ouro. Para obten??o de informa??es complementares da SAM, foram realizados c?lculos da Cobertura de Superf?cie, Constante Diel?trica e Espessura do tiol adsorvido no substrato de ouro. Ap?s esta etapa, a adi??o de ant?genos sol?veis de L. infantum sobre a SAM foi acompanhada por SPR. As t?cnicas de Voltametria C?clica e Espectroscopia de Imped?ncia Eletroqu?mica foram usadas para caracterizar a imobiliza??o do ant?geno. Ap?s constru??o do imunosensor, foram adicionados em sua superf?cie soros caninos positivos para Leishmaniose Visceral, evidenciando varia??o significativa no ?ngulo de SPR, mostrando excelente sensibilidade da t?cnica para detec??o da intera??o ant?geno-anticorpo. Por outro lado, a adi??o dos soros negativos n?o foi acompanhada com resposta significativa, concluindo-se tamb?m que o imunosensor apresentou boa especificidade contra anticorpos anti-L. infatum. Portanto, neste trabalho foi desenvolvido com sucesso um sensor empregando SPR para detec??o em tempo real de anticorpos anti-L. infatum, apresentando grande perspectiva como sistema de sensoriamento da Leishmaniose Visceral em ?reas end?micas. / Disserta??o (Mestrado) ? Programa de P?s-Gradua??o em Qu?mica, Universidade Federal dos Vales do Jequitinhonha e Mucuri, 2012. / ABSTRACT In this work, the development of an immunosensor for detection of anti-Leishmania infantum antibodies was performed. The principle of transduction used was the Surface Plasmon Resonance (SPR) and the sensor was constructed by covalent immobilization of soluble antigens of Leishmania infantum on self-assembled monolayers (SAMs) of 11-mercaptoundecanoic acid (11-MUA) which was activated by the mixture 100.0 mmol.L-1 1-ethyl-3 (3-dimethylaminopropyl) carbodiimide (EDC) and 150 mmol.L-1 N-hidroxisuccinimide (NHS). Cyclic Voltammetry and Dessortive Reduction by Differential Pulse Voltammetry techniques were employed in monitoring of SAM formation. Under optimized conditions, 1.0 mmol.L-1 of the 11-MUA in ethanolic solution and 24 hours were sufficient for the formation of a stable SAM on the gold surface. To obtain further information about the SAM, the Surface Coverage, Dielectric Constant and Thickness of the thiol film adsorbed on gold substrate were performed. After this step, the addition of soluble antigens?of L.?infantum?on the?SAM?was monitored?by SPR. Cyclic Voltammetry and Electrochemical Impedance Spectroscopy techniques were employed in characterization of antigen immobilization. After construction of immunosensor, positive canine serum for Visceral Leishmaniasis were added on its surface showing significant variation in the SPR angle, indicating excellent sensitivity of the technique for?antigen-antibody interaction detection. On the other hand, the addition of negative serum was not accompanied with a significant response, demonstrating that the immunosensor shows excellent specificity against anti-L infantum antibodies. Therefore, this work shows a successfully development of a SPR sensor for anti-L. infatum antibodies detection in real time, showing a great perspective as a sensing system of Visceral Leishmaniasis in endemic regions.
127

Produ??o de biodiesel por rotas et?licas e met?licas promovidas por irradia??o de micro ? ondas oriundas de um forno dom?stico n?o modificado

Miranda, S?vio Eduardo Oliveira 29 October 2011 (has links)
Submitted by Rodrigo Martins Cruz (rodrigo.cruz@ufvjm.edu.br) on 2015-02-19T13:34:46Z No. of bitstreams: 5 edu.pdf: 1793374 bytes, checksum: 659bf4622f25b099b1d7c3bd613d8f8a (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) / Approved for entry into archive by Rodrigo Martins Cruz (rodrigo.cruz@ufvjm.edu.br) on 2015-02-20T11:06:41Z (GMT) No. of bitstreams: 5 edu.pdf: 1793374 bytes, checksum: 659bf4622f25b099b1d7c3bd613d8f8a (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) / Made available in DSpace on 2015-02-20T11:06:41Z (GMT). No. of bitstreams: 5 edu.pdf: 1793374 bytes, checksum: 659bf4622f25b099b1d7c3bd613d8f8a (MD5) license_url: 52 bytes, checksum: 3d480ae6c91e310daba2020f8787d6f9 (MD5) license_text: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) license.txt: 2110 bytes, checksum: b4c884761e4c6c296ab2179d378436d4 (MD5) Previous issue date: 2013-02-20 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (Capes) / Neste trabalho est? descrito uma nova metodologia para a produ??o de biodiesel (?steres met?licos ou et?licos de ?cidos graxos) a partir do emprego de diversos ?leos vegetais na sua forma ?bruta?, assim como ?leos residuais oriundos de processo de fritura e tamb?m gordura animal (sebo) como material de partida. Al?m deste desafio, procurou-se realizar as rea??es de transesterifica??es em um processo acelerado por irradia??o das micro-ondas obtidas a partir de um forno de micro-ondas dom?stico, o qual n?o sofreu adapta??es, tais como: inser??o de um sistema de agita??o e tamb?m de refluxo, para ser utilizado em rea??es qu?micas. O primeiro passo do trabalho incluiu a utiliza??o dos diferentes ?leos vegetais brutos, isto ?, desprovidos de processo de refino e de degomagem, para a produ??o de biodiesel. Para tanto foi necess?rio o desenvolvimento de uma metodologia que permitisse a purifica??o desses ?leos vegetais brutos, pois estes podem conter subst?ncias, como a ?gua, os ?cidos graxos livres (AGL) e os ?steres de f?sforos (fosfat?dicos) que s?o inibidoras do processo de transesterifica??o. Na busca por uma t?cnica que permitisse a pr?via purifica??o desses ?leos vegetais, foram testados e obtidos excelentes resultados, quando foi realizada a sua filtra??o em s?lica gel 60 Mesh. A polaridade dessa s?lica oriunda dos grupos silan?is permitiu com grande ?xito a reten??o de AGL e dos ?steres de f?sforo, al?m do seu alto poder de adsor??o, reduzindo de maneira significativa o teor de ?gua presente nesses ?leos vegetais. O fator limitante para o emprego da s?lica gel comercial nos processos de purifica??o das diversas oleaginosas foi o seu alto custo, o que tornava invi?vel o processo de purifica??o. Ap?s diversos estudos e tentativas de encontrar um processo que substitu?sse a s?lica gel comercial anteriormente empregada, foi realizado a s?ntese de uma nova s?lica gel a partir do emprego de areia de constru??o e de carbonatos, sendo um processo simples e de baixo custo. Os resultados obtidos no processo de purifica??o dos ?leos vegetais brutos empregando s?lica gel ?sint?tica? foram similares aos da s?lica gel ?comercial?, o que levou o emprego desse processo de purifica??o de maneira sistem?tica no preparo de mat?ria-prima (reagentes) para posterior transesterifica??o. Os bons resultados permitiram testes dessa nova metodologia de purifica??o em ?leos e gorduras residuais (OGR) oriundos de processos de fritura. Nesses ?leos foram encontrados um n?mero bem maior de subprodutos (impurezas) que podem inibiriooooooo65t\azs NM de maneira parcial ou total o processo de transesterifica??o. Dessa forma, a purifica??o dos OGR tornou-se um grande desafio para a s?lica gel ?sint?tica?. Entre as impurezas contidas nesses ?leos residuais, podemos destacar os AGL, ?gua e os produtos oriundos da degrada??o oxidativa e t?rmica (per?xidos, alde?dos, cetonas, furanos, mon?meros c?clicos e n?o c?clicos) dos ?leos vegetais. Os OGR foram purificados com excelentes resultados por filtra??o sob s?lica gel ?sint?tica? em um processo realizado a temperatura ambiente. Al?m dos ?leos residuais puros, nesse processo foi obtida a gordura animal, a qual ficou retida sobre a s?lica sint?tica dentro do funil de filtra??o. Essa gordura animal foi posteriormente purificada por filtra??o a 60 ?C tamb?m em s?lica gel sint?tica e assim como o ?leo residual utilizada como material de partida na s?ntese de biodiesel. Vale ressaltar que os bons resultados alcan?ados no processo de purifica??o sob s?lica gel sint?tica e a necessidade crescente de mat?ria-prima (?leos vegetais), incentivou a amplia??o do programa de coleta de ?leo e gorduras residuais (OGR) na cidade de Diamantina/MG, intitulado como ?Doe Energia? e implantado em 2006. Tanto os ?leos vegetais brutos, como os ?leos residuais e a gordura animal purificados em s?lica gel sint?tica foram transesterificados a biodiesel (met?lico ou et?lico) em alcoolatos (metanolatos e etanolatos) previamente preparados ?in situ? a partir da solubiliza??o de NaOH ou KOH em metanol ou etanol. Neste processo ocorreu a adi??o do alcoolato sobre o material de partida, sendo a rea??o conduzida sob irradia??o de micro-ondas dom?stica a 240 W durante dez minutos e acompanhada por cromatografia em camada delgada (CCD). Os produtos da rea??o (biodiesel e glicerina) foram separados por decanta??o em funil de separa??o, sendo o biodiesel (et?lico ou met?lico) posteriormente lavado at? pH neutro, seco em Na2SO4 e purificados por destila??o a press?o reduzida. A caracteriza??o do biodiesel produzido foi realizada por m?todos espectrom?tricos como a RMN1H e 13C, al?m disso, o controle de qualidade do biodiesel produzido foi realizado empregando t?cnicas anal?ticas seguindo as normas preconizadas pela Ag?ncia Nacional de Petr?leo, G?s Natural e Biocombust?veis (ANP). A glicerina foi purificada, atrav?s de um pr?vio tratamento com adi??o de ?cido sulf?rico ou clor?drico, gerando o AGL, biodiesel e sulfatos ou cloretos de metais alcalinos como co-produtos. Alguns desses sais como o sulfato de s?dio foi posteriormente purificados por recristaliza??o e utilizados como dessecantes para o pr?prio biodiesel. A efici?ncia da metodologia empregando irradia??o de micro-ondas dom?stica, levou ao estudo do seu uso em rea??es in situ, ou seja, transesterifica??o direta das sementes e dos frutos de oleaginosas, tais como a soja e a mamona. Esse processo consiste em uma desidrata??o pr?via dos frutos ou sementes a uma temperatura de 80 ?C durante 8 horas. O alcoolato preparado foi adicionado sobre os frutos ou sementes triturados e secos e a mistura foi agitada com o aux?lio de um agitador mec?nico a 7500 rpm durante 10 minutos a temperatura ambiente, a fim de homogeneizar a mistura reacional. Essa mistura foi levada a um forno de micro-ondas dom?stico e irradiada a 240 W durante 10 minutos em um processo acompanhado por CCD. Ap?s esse per?odo a massa reacional foi filtrada sob v?cuo, a fim de eliminar o res?duo vegetal s?lido (torta). A solu??o resultante foi transferida para um funil de separa??o, onde ocorreu ap?s poucos minutos, a separa??o do biodiesel (fase superior) da glicerina (fase inferior) por simples decanta??o. Os produtos foram separados por decanta??o e tanto a glicerina como o biodiesel (et?lico ou met?lico) foram purificados e caracterizados. O rendimento em biodiesel foi de aproximadamente 96% no emprego de sementes de soja e de 97% empregando sementes de mamona. / Disserta??o (Mestrado) ? Programa de P?s-Gradua??o em Qu?mica, Universidade Federal dos Vales do Jequitinhonha e Mucuri, 2011. / ABSTRACT This work described a new methodology for the production of biodiesel (methyl or ethyl esters of fatty acids) from the use of various vegetable oils in its "raw" as well as waste oil from the frying process and also animal fat (tallow) as starting material. In addition to this challenge, we tried to carry out the reactions transesterification in a process accelerated by microwave irradiation obtained from a domestic microwave oven, which has not undergone changes, such as insertion of an agitation system and also reflux for used in chemical reactions. The first step of the work included the use of different crude oils, this is, devoid of the process of refining and degumming, for the production of biodiesel. For this purpose it was necessary to develop a methodology that allows the purification of crude vegetable oils, as they may contain different substances such as water, free fatty acids (FFA) and esters of phosphorus (Phosphatidic) which are inhibitors of the transesterification process. In the search for a technique that allowed the prior purification of vegetable oils have been tested and achieved excellent results when your filtration was performed on silica gel 60 Mesh. The polarity of this coming from the silica silanol groups with great success allowed the retention of FFA and phosphorus esters, in addition to its high adsorption, significantly reducing the water content present in these oils. The limiting factor for the commercial use of silica gel in the purification processes of other crops was the high cost, which made impossible the purification process. After several studies and attempts to find a process to replace the previously used commercial silica gel was carried out the synthesis of a new silica gel from the use of construction sand and carbonates, with a simple and low cost. The results obtained in the purification process of crude vegetable oils using silica gel "synthetic" were similar to those of silica gel "commercial", which led to the use of this purification process in a systematic manner in the preparation of raw materials (reagents) for subsequent transesterification. The good results allowed testing of this new method of purification of waste oils and fats (WOF) from the frying process. These oils have been found a much larger number of products (impurities) in a manner that can inhibit the partial or total transesterification process. Thus, the purification of WOF has become a major challenge for the silica gel "synthetic". Among the residual impurities contained in these oils, we can highlight the FFA, water and products from thermal and oxidative degradation (peroxides, aldehydes, ketones, furans, cyclic and non cyclic monomers) of vegetable oils. The WOF with excellent results were purified by filtration on silica gel "synthetic" in a process performed at room temperature. Besides the pure residual oils, this process was obtained animal fat, which was held on the synthetic silica into the filter funnel. This fat was then purified by filtration at 60 ?C also on silica gel and synthetic as well as the residual oil is also used as starting material in the synthesis of biodiesel. It is noteworthy that the good results achieved in the purification process in synthetic silica gel and the increasing need of raw material (vegetable oils) has encouraged the expansion of the program to collect waste oil and fats (WOF) in the Diamantina / MG city, titled as "Energy Donate" and implemented in 2006. Both crude vegetable oils, such as waste oils and animal fat purified on silica gel synthesis was transesterified biodiesel (methyl or ethyl) in alcoholates (metanolatos and ethanolate) previously prepared "in situ" from the solubilization of NaOH or KOH in methanol or ethanol. This process was the addition of alcoholates on the starting material, and the reaction was conducted under microwave irradiation of a 240 W home for ten minutes and accompanied by thin layer chromatography (TLC). The reaction products (biodiesel and glycerol) were separated by decanting funnel separation, and biodiesel (methyl or ethyl) subsequently washed until neutral, dried on Na2SO4 and purified by distillation at reduced pressure. The characterization of the biodiesel produced was performed by spectrometric methods such as RMN 1H and 13C, in addition, the quality control of biodiesel was carried out using analytical techniques following the standards recommended by the National Petroleum, Natural Gas and Biofuels Agency (ANP). The glycerin was purified through a previous treatment with sulfuric acid or hydrochloric acid, generating the FFA, biodiesel or chlorides and sulfates of alkali metals as co-product. Some of these salts such as sodium sulfate was further purified by recrystallization and used as desiccants for their own biodiesel. The efficiency of the methodology using a household microwave irradiation, led to the study of their use in reactions in situ, that is, direct transesterification of seeds and fruits of oilseeds such as soybeans and castor beans. This process consists of a prior dehydration of fruits or seeds at a temperature of 80 ?C for 8 hours. The alcoholates prepared was added on the fruits or seeds crushed and dried mixture was stirred with the aid of a mechanical stirrer at 7500 rpm for 10 minutes at room temperature in order to homogenize the reaction mixture. This mixture was brought to a domestic microwave oven and irradiated at 240 W for 10 minutes in a process monitored by TLC. After this time the reaction mass was filtered under vacuum to remove the solid waste plant (cake). The resulting solution was transferred to a separatory funnel, which occurred a few minutes, after the separation of biodiesel (upper phase) of glycerin (lower phase) by simple decantation. The products were separated by decantation and glycerin as much biodiesel (methyl or ethyl) have been purified and characterized. The yield of biodiesel was approximately 96% in the use of soybean and 97% employing castor beans.
128

Petrologia e geocronologia U-Pb do pl?ton gran?tico Serra da Rajada, por??o central do dom?nio Rio Piranhas - Serid?, Prov?ncia Borborema, NE do Brasil

Costa, Alan Pereira da 23 April 2015 (has links)
Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-07-25T19:35:27Z No. of bitstreams: 1 AlanPereiraDaCosta_DISSERT.pdf: 24726684 bytes, checksum: 6b4523ea74314d3a8b4944c8fbeef8ad (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-07-28T21:11:34Z (GMT) No. of bitstreams: 1 AlanPereiraDaCosta_DISSERT.pdf: 24726684 bytes, checksum: 6b4523ea74314d3a8b4944c8fbeef8ad (MD5) / Made available in DSpace on 2016-07-28T21:11:35Z (GMT). No. of bitstreams: 1 AlanPereiraDaCosta_DISSERT.pdf: 24726684 bytes, checksum: 6b4523ea74314d3a8b4944c8fbeef8ad (MD5) Previous issue date: 2015-04-23 / A atividade plut?nica ediacarana, relacionada a orog?nese Brasiliana/Pan-Africana, constitui uma das mais importantes fei??es geol?gicas na Prov?ncia Borborema, representada em sua extens?o por in?meros bat?litos, stocks e diques. O Pl?ton Gran?tico Serra da Rajada (PGSR), principal objeto desse estudo, situado na por??o central do Dom?nio Rio Piranhas-Serid? representa um exemplo dessa atividade, sendo objeto de estudos cartogr?fico, petrogr?fico, litogeoqu?mico e geocronol?gico. Suas rochas s?o individualizadas em duas f?cies, sendo a f?cies gran?tica descrita como monzogranitos constitu?dos por K-feldspato, plagiocl?sio (oligocl?sico-An23-24%), quartzo e biotita (m?fico principal), tendo como minerais acess?rios opacos, titanita, allanita, apatita e zirc?o. Clorita, mica branca e carbonato s?o minerais de altera??o. A f?cies dior?tica compreende rochas formadas por quartzo diorito contendo plagiocl?sio (fase mineral dominante), quartzo e K-feldspato. Biotita e anfib?lio s?o os minerais m?ficos dominantes, e titanita, minerais opacos, allanita, zirc?o e apatita s?o os acess?rios. Contudo, os trabalhos de cartografia geol?gica tamb?m identificaram na regi?o a presen?a de outras unidades litoestratigr?ficas, descritas como gnaisses e migmatitos indiferenciados com lentes de anfibolitos relacionados ao Complexo Caic? (Paleoproterozoica) e rochas metassedimentares do Grupo Serid? (Neoproterozoico) compostos por paragnaisses com lentes de calciossilic?ticas, muscovita quartzitos e biotita xistos (respectivamente forma??es Jucurutu, Equador e Serid?), os quais s?o as encaixantes para as rochas do PGSR. Ainda foram identificados diques de leucomicrogranito e de pegmatitos, ambos relacionados ao final do magmatismo Ediacarano, bem como dep?sitos col?vio-eluviais e aluvionares relacionados ao Ne?geno e Quatern?rio, respectivamente. Dados litogeoqu?micos, na f?cies gran?tica do PGSR, evidenciam rochas bastante evolu?das (SiO2 69% a 75%), rica em ?lcalis (Na2O+K2O ? 8,0%), empobrecidas em MgO (? 0,45%), CaO (? 1,42%) e TiO2 (? 0,36%) e teores moderados de Fe2O3t (2,16 a 3,53%). Apresentam natureza transicional entre metaluminosa e peraluminosa (predom?nio do ?ltimo) e possuem afinidade subalcalina/monzon?tica (c?lcio-alcalina de alto K). Diagramas de Harker mostram correla??es negativas em Fe2O3t, MgO e CaO, indicando fracionamento de m?ficos e plagiocl?sio. O espectro de ETR mostra enriquecimento dos ETR leves com rela??o aos ETR pesados (LaN/YbN = 23,70 a 0,23), com anomalia negativa no Eu (Eu/Eu* = 0,70 a 0,23), sugerindo fracionamento ou acumula??o na fonte de feldspatos (plagiocl?sio). A integra??o dos dados permite correlacionar ?s rochas do PGSR ?quelas referidas na literatura como Su?te C?lcio-Alcalina de Alto K Equigranular. Considera??es sobre as condi??es de cristaliza??o para as rochas do PGSR foram obtidas a partir da integra??o de dados petrogr?ficos e litogeoqu?micos, os quais indicaram atua??o de condi??es moderadas a elevadas de ?O2 (parag?nese mineral titanita + magnetita + quartzo), magma progenitor saturado em H2O (cristaliza??o precoce das biotitas), atua??o de processos tardi-magm?ticos de fluidos ricos em ?CO2, H2O e O2 causando altera??es em parte da assembleia mineral (carbonata??o e saussuritiza??o dos plagiocl?sio, cloritiza??o das biotitas e esfenitiza??o dos opacos). Condi??es de termobarom?tricas foram estimadas com base em par?metros geoqu?micos (Zr e P2O5), bem como por minerais normativos CIPW, com resultados mostrando temperatura m?nima de liquidus da ordem de 800?C e temperatura de solidus da ordem de 700?C. As press?es final/m?nima de cristaliza??o sugerem ser da ordem de 3 a 5 Kbar. A presen?a de minerais zonados (plagiocl?sio e allanita) associadas a dados litogeoqu?micos diagramas bi-log para Rb vs Ba e Rb vs Sr sugerem a atua??o da cristaliza??o fracionada como processo dominante na evolu??o magm?tica do PGSR. Estudos geocronol?gicos U-Pb e isot?picos Sm-Nd indicam, respectivamente, que o biotita monzogranito possui idade de cristaliza??o de 557?13 Ma, com idade modelo TDM de 2,36 Ga, tendo valor de eNd para a idade de cristaliza??o de -20,10, permitindo inferir fonte crustal paleoproterozoica para o magma. / The ediacaran plutonic activity related to the Brasilian/Pan-African orogeny is one of the most important geological features in the Borborema Province, represented along its extension by numerous batholiths, stocks, and dikes.The object of this study, the Serra Rajada Granitic Pluton (SRGP), located in the central portion of the Piranhas-Serid? River Domain is an example of this activity. This pluton has been the subject of cartographic, petrographic, geochronological and lithogeochemical studies and its rocks were characterized by two facies. First, the granitic facies were described as monzogranites consisting of K-feldspar, plagioclase (oligoclase - An23-24%), quartz and biotite (main mafic) and opaque minerals such as titanite, allanite, apatite, and zircon as accessories. Alteration minerals are chlorite, white mica and carbonate. Second, the dioritic facies consist of rocks formed by quartz diorite containing plagioclase (dominant mineral phase), quartz and K-feldspar. Biotite and amphibole are the dominant mafic minerals; and titanite, opaque minerals, allanite, zircon and apatite are the accessories. However, previous geological mapping work in the region also identified the presence of other lithostratigraphic units. These were described as gneisses and migmatites with undifferentiated amphibolite lenses related to the Caic? Complex (Paleoproterozoic) and metasedimentary rocks of the Serid? Group (Neoproterozoic) composed of paragneiss with calc-silicate lenses, muscovite quartzite and biotite schist (respectively, the Jucurutu formations, Equador and Serid?), the host rocks for the SRGP rocks. Leucomicrogranite and pegmatite dikes have also been identified, both related to the end of the Ediacaran magmatism and colluvial- eluvial and alluvial deposits related to Neogene and Quaternary, respectively. Lithogeochemical data on the SRGP granite facies, highlighted quite evolved rocks (SiO2 69% to 75%), rich in alkalis (Na2O+K2O ? 8.0%), depleted of MgO (? 0.45%), CaO (? 1.42%) and TiO2 (? 0.36%) and moderate levels of Fe2O3t (2.16 to 3.53%). They display transitional nature between metaluminous and peraluminous (predominance of the latter) with sub-alkaline/monzonitic (High K calcium-alkali) affinity. Harker diagrams show negative correlations for Fe2O3t, MgO, and CaO, indicating mafic and plagioclase fractionation. REE spectrum shows enrichment of LREE relative to heavy REE (LaN/YbN = 23.70 to 10.13), with negative anomaly in the Eu (Eu/Eu* = 0.70 to 0.23), suggesting fractionation or accumulation in the feldspars source (plagioclase). Data integration allows to correlate the SRGP rocks with those described as Calcium-Alkaline Suite of equigranular High K. The crystallization conditions of the SRGP rocks were determined from the integration of petrographic and lithogeochemical data. These data indicated intermediate to high conditions of ?O2 (mineral paragenesis titanite + magnetite + quartz), parent magma saturated in H2O (early biotite crystallization), tardi-magmatic processes of fluids rich in ?CO2, H2O and O2 causing part of the mineral assembly to change (plagioclase carbonation and saussuritization, biotite chloritization and opaques Sphenitization). Thermobarometrical conditions were estimated based on geochemical parameters (Zr and P2O5) and CIPW normative minerals, with results showing the liquidus minimum temperature of about800?C and the solidus temperature of approximately 700?C. The final/minimum crystallization pressure are suggested to be between 3 and 5 Kbar. The presence of zoned minerals (plagioclase and allanite) associated with lithogeochemical data in bi-log diagrams for Rb vs. Ba and Rb vs. Sr suggest the role of fractional crystallization as the dominant process in the magmatic evolution of SRGP. U-Pb Geochronological and Sm-Nd isotope studies indicated, respectively, the crystallization age of biotite monzogranite as 557 ? 13 Ma, with TDM model age of 2.36 Ga, and ?Nd value of -20.10 to the crystallization age, allowing to infer paleoproterozoic crustal source for the magma.
129

Estudo da formula??o de massas cer?micas provenientes da regi?o do Serid?-RN para fabrica??o de telhas

Andrade, Felipe Lira Formiga 06 March 2009 (has links)
Made available in DSpace on 2014-12-17T14:57:50Z (GMT). No. of bitstreams: 1 FelipeLFA.pdf: 4959653 bytes, checksum: 0da7f126d56ee6a849bfaf9a5d53da1d (MD5) Previous issue date: 2009-03-06 / Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico / This work has for objective study compared the characteristics and technological properties of ceramic bodies from the region of Serid?-RN. The region under study has identified 23 cities where they were 80 ceramics industries. To define the universe of search, there was a survey of pottery that are part of APL Serid? next to the IEL. The characteristics and operating conditions of ceramics industries of the region were identified through a socio-economic questionnaire applied locally, which addressed issues such as: profiles of companies, production process etc. The analysis of information collected from 24 companies identified in seven cities shows that the vast majority of industries is small, with family structure, obsolete equipment and labo, little qualified. Most of the pottery works with low technical knowledge, poor control of the production process and product technology. The raw collected were submitted to analysis of X ray diffraction, chemical composition, termical analysis, particle size distribution and plasticity. Then were produced five formulations and made by uniaxial pressure at 25 MPa for firing in temperatures varying from 850 to 1050 ?C. The firing technological properties evaluated were: mass loss to fire, lineal shrinkage, apparent density, apparent porosity, water absorption and flexural strength (3 points). The results indicated that the raw materials from the region have significant similarities in the composition chemical and mineralogical. Furthermore, it indicates the possibility of the use of cycles of firing faster and efficient than the current, limited to some clay mass burning of certain conditions / Este trabalho teve como objetivo estudar comparativamente as caracter?sticas e propriedades tecnol?gicas de massas cer?micas para telhas da regi?o do Serid?-RN. A Regi?o em estudo possui 23 munic?pios onde foram identificadas 80 ind?strias cer?micas. Para defini??o do universo da pesquisa, fez-se um levantamento das olarias que fazem parte da APL Serid? junto ao IEL do Estado. As caracter?sticas e condi??es de funcionamento das ind?strias cer?micas da regi?o foram identificadas atrav?s de um question?rio s?cio-econ?mico aplicado in loco, que abordava aspectos como: perfil das empresas, processo produtivo etc. A an?lise das informa??es coletadas em 23 empresas identificadas em sete munic?pios permite concluir que a grande maioria das ind?strias ? de pequeno porte, com estrutura familiar, equipamentos obsoletos e m?o-de-obra pouco qualificada. Grande parte das olarias opera com baixo conhecimento t?cnico, prec?rios controles do processo produtivo e tecnol?gico dos produtos. As mat?rias-primas coletadas foram submetidas a ensaios de difra??o de raios X, composi??o qu?mica, an?lise t?rmica, distribui??o de tamanho de part?culas e plasticidade. Em seguida foram produzidas cinco formula??es e confeccionados corpos-de-prova por prensagem uniaxial a 25 MPa para queima variando de 850 ?C a 1050?C. As propriedades tecnol?gicas de queima avaliadas foram: perda de massa ao fogo, retra??o linear, massa espec?fica aparente, porosidade aparente, absor??o de ?gua e carga de ruptura ? flex?o (3 pontos). Os resultados indicaram que as mat?rias-primas provenientes da regi?o apresentam significativas semelhan?as quanto ? composi??o qu?mica e mineral?gica. Al?m disso, indica-se a possibilidade da utiliza??o de ciclos de queima mais r?pidos e eficientes que os atuais, limitando algumas massas argilosas para certas condi??es de queima
130

Estudo das vari?veis de processamento das mat?rias-primas da regi?o do crato - ce na fabrica??o de produtos cer?micos por extrus?o e por prensagem

Santos, Getulio de Moura 10 July 2010 (has links)
Made available in DSpace on 2014-12-17T14:57:55Z (GMT). No. of bitstreams: 1 GetulioMS.pdf: 1235965 bytes, checksum: 2c47ca0471a5470d046cd558e9c9cca4 (MD5) Previous issue date: 2010-07-10 / The limits to inform is about the character stico of basic, quimica, mineralogical and mechaniques of matlaughed material used in the manufacturing process the product certified in economic region the Cariri, specifically in the city of Crato, Cear? state, motivated the development of this work, since in this region the exist ing economic context that a general appear as important in the production chains. Were made twentyfive soils-test specimen collection and the study was performed to differentiate the mat laugh materials of variaveis processing of mathing raw materials in the factory The product mica monkeys by extrusion and pressing. The results were obtained ap s as analyzes: grain size, index of plasticity, fluoresce incidence X-ray difration the X-ray, and analyzes thermicals and properties technological. through s of curves gresifica returned to was a comparison between the retro the linear, absorb to water, porosity and bulk density. the results show that the excellent distribution and character acceptable available for the processing of the structure color dark red. needing, therefore, of the mixture of a less plastic clay with thick granulation, that works as plasticity reducer. In spite of the different resignation forms for prensagem and extrusion, the characteristics of absorption of water and rupture tension the flexing was shown inside of the patterns of ABNT / A limita??o de informa??es sobre as caracter?sticas f?sicas, qu?micas, mineral?gicas e mec?nicas da mat?ria-prima usada no processo de fabrica??o dos produtos cer?micos na regi?o do Cariri, mais precisamente na cidade do Crato, estado do Cear?, motivou o desenvolvimento deste trabalho, visto que nesta regi?o existem cer?micas que num contexto geral figuram como cadeias produtivas importantes no estado. Foram confeccionados vinte e cinco corpos-de-prova da amostra coletada para cada m?todo de conforma??o e foi realizado o estudo das vari?veis de processamento das mat?riasprimas na fabrica??o de produtos cer?micos por extrus?o e prensagem. Os resultados foram obtidos ap?s as an?lises de: granulometria, ?ndice de plasticidade, fluoresc?ncia de raios X, difra??o de raios X, an?lises t?rmicas e propriedades tecnol?gicas. Atrav?s das curvas de gresifica??o obteve-se um comparativo entre a retra??o linear de queima, absor??o de ?gua, porosidade e massa espec?fica aparente. Os resultados mostram que a mat?ria-prima tem excelente distribui??o e caracter?sticas aceit?veis para o processamento de pe?as estruturais de cor escura a vermelha, necessitando, pois, da mistura de uma argila menos pl?stica com granula??o grossa, que funciona como redutor de plasticidade. Apesar das diferentes formas de conforma??o por prensagem e extrus?o, as caracter?sticas de absor??o de ?gua e tens?o de ruptura a flex?o mostrou-se dentro dos padr?es da ABNT

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