Eletroforese capilar acoplada à espectrometria com plasma: uma ferramenta eficiente para a especiação

The most important features of the CE-ICP hyphenation, as well as its advantages and drawbacks as a tool for speciation are discussed. The fundamental principles of capillary electrophoresis and inductively coupled plasma mass spectrometry are also presented. Some applications involving different designs proposed in the literature to couple CE and ICP system for elemental speciation are reviewed.

Fluidos supercríticos em química analítica. II. Cromatografia com fluido supercrítico: instrumentação

The first paper in this series discussed the basic theory involved in supercritical fluid chromatography (SFC) and how the technique progressed from gas and liquid chromatography. The first SFC instruments were simple adaptations of the commercially available liquid chromatographs with packed columns followed by modifications in gas chromatographs using open tubular capillary columns. In this paper, the most important aspects regarding instrumentation are covered, including practical, simple, and the most important, inexpensive solutions to build a home-made SFC system.

Fluidos supercríticos em química analítica. III.: aplicações

The first two papers in this series described the basic theory involved in supercritical fluid chromatography (SFC), how the technique evolved from gas and liquid chromatography and how the instrumentation was developed. Over the last two years, a commercial, dedicated packed-column SFC/MS instrument appeared on the market. The SFC continues to grow in use, with fundamental developments, coupled with a steady rise in the number of industrial users and applications.

Synthesis, characterization and thermal behaviour of solid-state compounds of benzoates with some bivalent transition metal ions

Solid-state MBz compounds, where M stands for bivalent Mn, Fe, Co, Ni, Cu and Zn and Bz is benzoate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The procedure used in the preparation of the compounds via reaction of basic carbonates with benzoic acid is not efficient in eliminating excess acid. However the TG-DTA curves permitted to verify that the binary compounds can be obtained by thermosynthesis, because the benzoic acid can be eliminated before the thermal decomposition of these compounds. The results led to information about the composition, dehydration, thermal stability, thermal decomposition and structure of the isolated compounds. On heating, these compounds decompose in two (Mn, Co, Ni, Zn) or three (Fe, Cu) steps with formation of the respective oxide (Mn3O4, Fe2O3, Co3O4, NiO, CuO and ZnO) as final residue. The theoretical and experimental spectroscopic studies suggest a covalent bidentate bond between ligand and metallic center.

Terminologia para as técnicas analíticas de eletromigração em capilares

This is a contribution that presents a translation of the work "Terminology for Analytical Capillary Electromigration Techniques" by Riekkola and collaborators (Pure Appl. Chem., Vol. 76, No. 2, 443-451, 2004) from IUPAC© for the Portuguese Language. Additional terms that had not been defined in native Portuguese were included for the benefit of the local community. Additional notes were also included to clarify some important concepts and to highlight the differences between techniques.

Microssistemas de análises químicas: introdução, tecnologias de fabricação, instrumentação e aplicações

The amazing world of micro total analysis systems has provided a true revolution in analytical chemistry in recent years. The application of the microfluidic devices for chemical and biochemical processing has attracted considerable interest due to its advantages such as reduced sample and reagent consumption, processing time, energy, waste, cost, and portability. The aim of the present report is to disseminate the state of the art related to the miniaturization science in Analytical Chemistry. Historical progress, microfabrication technologies, required instrumentation and applications of the mTAS are presented in the current article, with special attention to the Brazilian contributions.

Seqüenciamento de peptídeos usando espectrometria de massas: um guia prático

This paper introduces the basics of peptide mass spectra interpretation applied to proteomics and is directed to chemists, biochemists and biologists. The manuscript presents a well detailed protocol aiming to serve as a first choice guide for understanding peptide sequencing. The tutorial was elaborated based on both a thorough bibliographic revision and the author's experience. In order to prove the applicability of the proposed guide, spectra obtained on different instruments have been successfully interpreted by applying the presented rational.

Eletroforese capilar acoplada à espectrometria de massas (CE-MS): vinte anos de desenvolvimento

CE-MS has been increasingly used for analysis of a vast array of compounds. This article reviews the different electrophoretic modes, interfaces and mass analyzers that are commonly used in the CE-MS coupling, as well as the technique advantages and performance characteristics. A large compilation of CE-MS applications is also presented. Therefore, this review is both a guide for beginners and a collection of key references for people who are familiar to the technique. Furthermore, this is the first CE-MS review published in a Brazilian journal and marks the installation of the first two commercial CE-MS units in Sao Paulo State.

Hidrólise de celulose por catalisadores mesoestruturados NiO-MCM-41 e MoO3-MCM-41

This study was carried out to synthesize, characterize and evaluate the application of mesoestruturated catalysts MCM-41, 5%MoO3-MCM-41 and 5%NiO-MCM-41 in the hydrolysis of microcrystalline cellulose. XRD results indicate that the phase of mesoporous MCM-41 was obtained and that the introduction of metal oxides did not affect this mesoporous phase. About the heterogeneous hydrolysis reaction, it was observed that the increase in temperature results in a higher concentration of glucose and the catalyst 5%MoO3-MCM-41 provides the highest concentrations of glucose.

Efeitos ópticos - eletrônicos de solventes nas polarizabilidades eletrônicas do íon Ni2+ no complexo [Ni(C3H4N2)6](CF3SO3)2

Polarizabilidades eletrônicas foram determinadas para o sal de tifluorometanosulfonato de níquel e para o complexo com imidazol, em soluções de metanol e de acetonitrila. A partir dos espectros eletrônicos, registrados numa concentração de 10-3 mol L-1 e pelo uso de um programa SIMP2FOS para o cálculo da força do oscilador experimental e POLAZ-F para o cálculo das polarizabilidades eletrônicas, foi possível perceber a distinta influência dos solventes na deformação da nuvem eletrônica do níquel (II).

Synthesis and characterization of Fe(III)-doped ceramic membranes of titanium dioxide and its application in photoelectrocatalysis of a textile dye

Pure and Fe(III)-doped TiO2 suspensions were prepared by the sol gel method with the use of titanium isopropoxide (Ti(OPri)4) as precursor material. The properties of doped materials were compared to TiO2 properties based on the characterization by thermal analysis (TG-DTA and DSC), X-ray powder diffractometry and spectroscopy measurements (FTIR). Both undoped and doped TiO2 suspensions were used to coat metallic substrate as a mean to make thin-film electrodes. Thermal treatment of the precursors at 400ºC for 2 h in air resulted in the formation of nanocrystalline anatase TiO2. The thin-film electrodes were tested with respect to their photocatalytic performance for degradation of a textile dye in aqueous solution. The plain TiO2 remains as the best catalyst at the conditions used in this report.

Avaliação da percepção de discentes do curso médico acerca do estudo anatômico

O presente trabalho objetivou conhecer a percepção dos alunos de Medicina sobre o estudo anatômico, para proposição de medidas que melhorem a aprendizagem dessa disciplina. Trata-se de estudo transversal com abordagem quantitativa e análise descritiva. Os dados foram coletados por meio de um questionário semiestruturado aplicado aos alunos do primeiro, segundo, terceiro, quinto e sexto períodos do curso médico. Para a maioria dos discentes, a aula expositiva facilita o aprendizado em Anatomia, ao passo que o grande número de nomes para memorizar foi apontado como principal fator dificultador. Grupo preponderante utiliza livros-texto e livro atlas, raramente tendo contato com peças naturais, e 82,59% dos acadêmicos não se sentem satisfeitos com o seu conhecimento anatômico. Portanto, no contexto atual de aumento da carga curricular do curso médico e redução do tempo dispensado à Anatomia, surge o desafio de examinar a evolução do currículo do curso médico observando a inserção da Anatomia neste processo. É necessário buscar um equilíbrio entre detalhe e segurança, assimilação e aplicabilidade da Anatomia, tendo em vista os diferentes métodos utilizados para o aprendizado da ciência anatômica.

Estimativa da produção anual de serapilheira dos bosques de mangue no Furo Grande, Bragança-Pará

As condições ambientais de determinado local podem influenciar a produtividade dos manguezais. Assim, este estudo estimou a produção total e dos componentes da serapilheira no Furo Grande, Bragança, PA. Este estudo compreendeu quatro ciclos anuais (julho/2000 a agosto/2004) em três sítios. Foram instaladas sete cestas em cada sítio ao longo de uma transecção de 140 m, com intervalos de 20 m. Cada cesta possuía uma área útil de 1 m², com tela de 1 mm², suspensa acima do nível das marés de sizígia. O material acumulado nas cestas foi coletado mensalmente, separado em folha, flor, fruto, estípula, galho e miscelânea, sendo posteriormente secado a 70 ºC até alcançar peso constante. A produção média dos quatro anos foi de 9,85 t.ha-1.ano-1 no sítio 1, 6,41 t.ha-1.ano-1 no sítio 2 e 5,99 t.ha-1.ano-1 no sítio 3, cuja comparação apresenta diferença significativa entre os sítios 1 e 3 (H=7,53; gl=2; p<0,05). Em suma, os resultados apontaram que a folha foi o componente de maior produtividade e, juntamente com a flor, teve pico na estação seca, o que parece favorecer uma economia de energia para o investimento em reprodução, enquanto a maior produção de fruto foi na estação chuvosa, promovendo a dispersão de propágulos e, conseqüentemente, a renovação e manutenção dessas florestas.

Planting density and initial growth of two tree species adapted to the semi-arid region

Planting densities influence several aspects of forest formation, including management practices, timber yield, quality, and extraction, and consequently its production costs. The objective of this study was to evaluate Mimosa caesalpiinifolia and Gliricidia sepium growth as a function of planting density (400, 600, 800, 1000, and 1200 plants ha-1) and plant age. The species were evaluated every 90 days for plant height (PH), crown diameter (CD) and root collar diameter (RCD) (10 cm above the ground), with the first evaluation performed at 90 days and the last at 720 days. When plants were one year of age and beyond, evaluations were conducted also for stem diameter at breast height (DBH) (1.30 m above the ground). A randomized block design with split-plots and three replicates was adopted. Species were assigned to plots, planting densities were assigned to subplots, and evaluation ages were assigned to subsubplots. The four traits in both species had their values decreased as planting density increased, but continually increased as plant age increased. For PH and RCD there was an alternation between species superiority, with gliricidia being superior to sabiá at some ages, while the opposite occurred at other ages. As to CD the species only differed in the last measurement, gliricidia being superior. With regard to DBH, gliricidia was superior starting from the second measurement. There was an effect of the species × ages interaction for the four traits and also an effect of the densities × ages interaction for CD and DBH.

Tratamento de águas residuárias de fecularia por meio de lagoas de estabilização

Embora o uso de lagoas de tratamento seja uma tecnologia amplamente conhecida e utilizada para resíduos orgânicos, no caso específico dos resíduos líquidos da industrialização da mandioca, as experiências são reduzidas. Assim, o objetivo deste trabalho foi de avaliar a eficiência na redução da carga poluidora de lagoas de tratamento de resíduos líquidos de fecularia. Para tanto, foram coletadas amostras na entrada do sistema e em cada uma das sete lagoas da Fecularia Horizonte, em Marechal Cândido Rondon - PR, no período de maio a setembro de 2004. Os seguintes parâmetros foram avaliados: Demanda Bioquímica de Oxigênio (DBO), Demanda Química de Oxigênio (DQO), Sólidos Totais (ST), Sólidos Fixos (SF), Sólidos Voláteis (SV), N-NH4+, Condutividade Elétrica (CE), Fósforo (P), Cloretos (CL-) e pH. O sistema promoveu redução de 96,3% de DQO e 96,4% de DBO, e fósforo e sólidos apresentaram comportamento semelhante. Já N-NH4+, CL- e CE oscilaram durante o sistema com redução, sobretudo nas lagoas de polimento.