Made available in DSpace on 2014-12-17T15:42:08Z (GMT). No. of bitstreams: 1
GenicksonBC_DISSERT.pdf: 3221273 bytes, checksum: 93f5a94a8d409de3a6c9189089010e14 (MD5)
Previous issue date: 2012-02-29 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / This work involved the synthesis, characterization and proposing the molecular
structure of coordination compounds involving ligands pyrazine-2-carboxamide (PZA) and 4-
hydrazide acidic pyridine carboxylic (INH) and metals of the first transition series (M = Co2+,
Ni2+ and Cu2+). For the characterization of the compounds used were analytical techniques
such as infrared absorption spectroscopy average (FT-IR) molar conductivity measurements,
CHN elemental analysis, EDTA Complexometric, measurement of melting point, X-ray
diffraction by powder method, Thermogravimetry (TG) and Differential Thermal Analysis
(DTA) and Simultaneous Differential Scanning Calorimetry (DSC). The absorption spectra in
the infrared region suggested that the ligand coordination to the metal center occurs through
the carbonyl oxygen atom and nitrogen alpha pyrazine ring to those complexes formed with
PZA. For INH complexes with metal-ligand coordination is through the carbonyl oxygen and
nitrogen of the terminal hydrazide grouping. The conductivity measurements of the
complexes in aqueous solution they suggest to all behavior of the type 1:2 electrolytes, and
conduct of non-electrolytes in acetonitrile. The results obtained by CHN elemental analysis
and EDTA Complexometric allowed to infer the stoichiometry of the compounds synthesized.
For all of the complexes obtained was possible to record the melting points, neither of which
melted near the melting temperature of the free ligands. The X-ray diffraction showed that the
complexes of pyrazinamide exhibited diffraction lines, suggesting that these compounds are
crystalline, while compounds of isoniazid, with the exception of cobalt, exhibited diffraction
lines, indicating that they are crystalline. The results from the TG-DTA and DSC allowed
information regarding the dehydration and thermal decomposition of these complexes / Este trabalho consistiu na s?ntese, caracteriza??o e proposi??o da estrutura molecular
de compostos de coordena??o envolvendo os ligantes pirazina-2-carboxamida (PZA) e 4-
hidrazida ?cida piridincarbox?lica (INH) e os metais da primeira s?rie de transi??o (M = Co2+,
Ni2+ e Cu2+). Para a caracteriza??o dos compostos foram utilizadas t?cnicas de an?lise como:
Espectroscopia de absor??o no Infravermelho m?dio (FT-IR), medidas de condutividade
molar, An?lise Elementar de CHN, complexometria com EDTA, medidas do ponto de fus?o,
Difra??o de raios-X pelo m?todo do p?, Termogravimetria (TG) e An?lise T?rmica
Diferencial (DTA) simult?nea e Calorimetria Explorat?ria Diferencial (DSC). Os espectros de
absor??o na regi?o do infravermelho sugerem que a coordena??o do ligante ao centro
met?lico ocorreu atrav?s do ?tomo de oxig?nio carbon?lico e do nitrog?nio alfa do anel
piraz?nico para os complexos formados com a PZA. Para os complexos com a INH a
coordena??o ligante-metal se d? pelo oxig?nio da carbonila e nitrog?nio terminal do
grupamento hidrazida. As medidas de condutividade dos complexos em solu??o aquosa
sugerem para todos eles comportamento de eletr?litos do tipo 1:2; e comportamento de n?o
eletr?litos em acetonitrila. Os resultados obtidos pela an?lise elementar de CHN e
complexometria com EDTA permitiram inferir a estequiometria dos compostos sintetizados.
Para todos os complexos obtidos foi poss?vel registrar os pontos de fus?o, sendo que nenhum
deles fundiu pr?ximo da temperatura de fus?o dos ligantes livres. Os difratogramas de raios-X
mostraram que os complexos da pirazinamida apresentaram linhas de difra??o, sugerindo que
estes compostos s?o cristalinos, enquanto os compostos da isoniazida, com exce??o ao de
cobalto, apresentaram linhas de difra??o, indicando que os mesmos s?o cristalinos. Os
resultados a partir das curvas TG-DTA e DSC permitiram informa??es a respeito da
desidrata??o e decomposi??o t?rmica destes complexos
| Identifer | oai:union.ndltd.org:IBICT/oai:repositorio.ufrn.br:123456789/17717 |
| Date | 29 February 2012 |
| Creators | Carvalho, Genickson Borges de |
| Contributors | CPF:31482015404, http://lattes.cnpq.br/2959800336802498, Silva, Ademir Oliveira da, CPF:16225422404, http://lattes.cnpq.br/3511004608337461, Oliveira, Otom Anselmo de, CPF:03936872449, http://lattes.cnpq.br/7903084274135177, Silva, Henrique Eduardo Bezerra da, CPF:48102288434, http://lattes.cnpq.br/2722164837738303, Moura, Maria de F?tima Vit?ria de |
| Publisher | Universidade Federal do Rio Grande do Norte, Programa de P?s-Gradua??o em Qu?mica, UFRN, BR, F?sico-Qu?mica; Qu?mica |
| Source Sets | IBICT Brazilian ETDs |
| Language | Portuguese |
| Detected Language | English |
| Type | info:eu-repo/semantics/publishedVersion, info:eu-repo/semantics/masterThesis |
| Format | application/pdf |
| Source | reponame:Repositório Institucional da UFRN, instname:Universidade Federal do Rio Grande do Norte, instacron:UFRN |
| Rights | info:eu-repo/semantics/openAccess |
Page generated in 0.002 seconds