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Química Nova, Volume: 21, Número: 4, Publicado: 1998
  • Editorial

    Andrade, Jailson B. de
  • Determinação dos hidrocarbonetos saturados e policíclicos aromáticos presentes no material particulado da atmosfera amazônica Artigo

    Vasconcellos, Pérola de Castro; Artaxo, Paulo Eduardo; Ciccioli, Paulo; Cecinato, Angelo; Brancaleoni, Enzo; Frattoni, Massimiliano

    Resumo em Inglês:

    It was identified and quantified several organic compounds in the atmosphere of a site into Amazon Basin with high impact of biomass burning emission. It was important to know the particulate matter composition with respect to n-alkanes and PAH associated with the particulate matter because they provided indication on the main sources contributing to airborne particles, the contribution of natural vs. man-made emission and the aging of the particles. The main classes of compounds observed were n-alkanes, PAH and nitro-PAH. It was observed the formation of nitro-PAH from photochemical reactions. The aerosol mass concentration is mainly associated with fluoranthene, pyrene and benzo(ghi)perylene. Environmental and direct emissions samples (flaming and smoldering) were collected and analysed.
  • Synthesis, characterization and thermal decomposition of [Pd2 (C²-dmba) (µ-SO4) (SO2)2]

    Caires, Antonio Carlos Fávero; Mauro, Antonio Eduardo

    Resumo em Inglês:

    The bridged sulphate complex [Pd2 (C²,dmba) (µ-SO4) (SO2)2] has been obtained by reacting a saturated solution of SO2 in methanol and the cyclometallated compound [Pd(C²,N-dmba)(µ-N3)] 2; (dmba = N,N-dimethylbenzylamine), at room temperature for 24 h. Reaction product was characterized by elemental analysis, NMR comprising 13C{¹H} and ¹H nuclei and I.R. spectrum's measurements. Thermal behavior has been investigated and residual products identified by X-ray powder diffraction.
  • Ácido ent-16alfa,17-diidroxicauran-19-óico isolado de Ouratea semiserrata e os desafios estereoquímicos dos carbonos quirais C-4 e C-16 Artigo

    Velandia, Javier Rincón; Carvalho, Mário Geraldo de; Braz-Filho, Raimundo

    Resumo em Inglês:

    Phytochemical investigation of the leaves and branches of a specimen of Ouratea semiserrata led to the isolation and characterization of ent-16alpha,17-dihydroxykauran-19-oic acid, along with other natural products. This diterpenoid and its derivatives were used to unambiguous ¹H and 13C chemical shifts assignments and to indicate some mistake data described in the literature as consequence mainly of the stereochemicals of the chiral carbons C-4 and C-16. The HRMS spectra were also analysed.
  • Emprego de nebulizador pneumático de ICP-MS como câmara de diluição em sistemas de injeção em fluxo para determinações multielementares Artigo

    Gomes Neto, José Anchieta; Silva, José Bento B.; Rodrigues Neto, Renato; Curtius, Adilson José; Souza, Ivan G.

    Resumo em Inglês:

    An automatic dispenser based on a flow-injection system used to introduce sample and analytical solution into an inductively coupled plasma mass spectrometer through a spray chamber is proposed. Analytical curves were constructed after the injection of 20 to 750 µL aliquots of a multielement standard solution (20.0 µg L-1 in Li, Be, Al, V, Cr, Mn, Ni, Co, Cu, Zn, As, Se, Sr, Ag, Cd, Ba, Tl, Pb) and the acquisition of the integrated transient signals. The linear concentration range could be extended to ca. five decades. The performance of the system was checked by analyzing a NIST 1643d reference material. Accuracy could be improved by the proper selection of the injected volume. Besides good precision (r.s.d. < 2%), the results obtained with the proposed procedure were closer to the certified values of the reference material than those obtained by direct aspiration or by injecting 125 µL of several analytical solutions and samples.
  • Análise das isotermas de adsorção de Cu(II), Cd(II), Ni(II) e Zn(II) pela N-(3,4-dihidroxibenzil) quitosana empregando o método da regressão não linear Artigo

    Klug, Marilene; Sanches, Maria N. M.; Laranjeira, Mauro C. M.; Fávere, Valfredo T.; Rodrigues, Clovis A.

    Resumo em Inglês:

    Adsorption of Cu(II), Ni(II), Pb(II) and Zn(II) ions from aqueous solutions by N-(3,4-dihydroxybenzyl) chitosan have been carried out. The Langmuir (L), Freundlich (F), Langmuir - Freundlich (LF), Redlich-Peterson (RP) and Tóth (T) adsorption isotherms models have been applied to fit the experimental data. Nonlinear regression computational program "Enzefitte", which is a library of the more commonly used adsorption isotherm equations for obtaining tabular outuput suitable for plotting theoretical of fitted isotherms, has been used to estimate the adsorption parameters. These parameters were used to calculate the amount adsorbed q calc., a function of concentration (C).
  • Determinações multi-elementares de metais, Sulfato e Cloreto em amostras de águas por espectrometria de massas com fonte de plasma (ICP-MS) Artigo

    Menegário, A. A.; Giné, M. F.

    Resumo em Inglês:

    The multi-element determination of Al, Cr, Mn, Ni, Cu, Zn, Cd, Ba, Pb, SO4= and Cl- in riverine water samples was accomplished by inductively coupled plasma mass spectrometry (ICP-MS). The sample passed through a column containing the anionic resin AG1-X8 and the metals were determined directly. The retained anionic species were eluted and SO4= and Cl- were determined at m/z 48 and 35 correspondent to the ions SO+ and Cl+ formed at the plasma. Accuracy for metals was assessed by analysing the certified reference TM-26 (National Water Research Institute of Canada). Results for SO4= and Cl- were in agreement with those obtained by turbidimetry and spectrophotometry. LOD's of 0.1 µg l-1 for Cd, Ba and Pb; 0.2 µg l-1 for Al, Mn and Cu; 0.5 µg l-1 for Cr; 0.9 for Zn; 2.0 µg l-1for Ni , 60 µg l-1 for S and 200 µg l-1 Cl were attained.
  • Comparação de dois tipos de amostragem de chuva: deposição total e deposição apenas úmida em àrea costeira tropical Artigo

    Campos, Vânia P.; Costa, Angela C. A.; Tavares, Tania M.

    Resumo em Inglês:

    In a tropical coastal area. During 6 months the composition of rain samples collected simultaneously over 24h with an open collector and with an automatic opened collector (KFA - J¸lich Type) at 500m of the Atlantic coastline of Salvador were compared. All average concentrations were higher for the "total" samples than for the "wet only" samples, except for hydrogen ions, nitrate and ammonium.
  • Influência de efluentes têxteis e alimentícios sobre o metabolismo e propriedades físicas e químicas do rio Piauitinga (Sergipe) Artigo

    Andrade, Regina Célia Bastos de; Souza, Marcelo Friederichs Landim de; Couto, Erminda da Conceição Guerreiro

    Resumo em Inglês:

    Metabolic rates were determined by dissolved oxigen changes in light and dark bottles, filled with river water and after input of mixed effluent concentrations. In another experiment, dissolved inorganic nutrients, chlorophyll-alpha and other physico-chemical parameters were analyzed. Water column showed higher decomposition than production rates. Waste inputs increased primary production rates, but in higher concentrations forced the system to heterotrophy. The natural richness of macrophytes and macroalgae could be limiting the phytoplanktonic production by phosphorus assimilation. Observation of the nitrogenated inorganic nutrients suggest that the natural pelagic system is directed to nitrification. Mixed waste input inverted this trend, toward denitrification.
  • Propriedades texturais e catalíticas de óxidos de ferro contendo cromo e cobre Artigo

    Souza, Marluce Oliveira da Guarda; Quadro, Emerentino Brazil; Rangel, Maria do Carmo

    Resumo em Inglês:

    Chromium and copper-doped hematites were prepared with the aim of studying the synergistic effect of these dopants on the textural and on the catalytic properties of the iron oxides towards the high temperature shift reaction. It was found that the most active catalysts were those with the highest amount of copper. They had the Fe(II)/Fe(III) ratio near the stoichiometric value of magnetite, the highest surface areas under the reactional atmosphere and the greatest tendency to produce the active form; they also were poorly crystalline solids. The best performance was shown by the catalyst with Fe/Cu=10, heated at 300ºC. It can thus be concluded that copper acts both as textural and structural promoter in these catalysts.
  • X-ray fluorescence determination of adsorbed copper on activated charcoal after glycerin complexation

    Bueno, Maria Izabel Maretti Silveira; Amaral, Lêda Cristina do

    Resumo em Inglês:

    X-This work shows an alternative method to copper determination by X-Ray Fluorescence (XRF). Since copper concentration in natural waters is not enough to reach XRF detection limit, a liquid-solid preconcentration procedure was proposed. Glycerin was used to complex the metal increasing its adsorption on activated charcoal. The solid phase was used to XRF determination. Several parameters were evaluated, such as, the complexation pH, the charcoal adsorption limit and the glycerin concentration. The interferences are lead and bismuth and the sensitivities decreased in the order Cu2+, Bi3+ and Pb2+. The advantages of the method are its simplicity, low cost and low spectral interference.
  • Estimativa da entalpia de decomposição (deltaD Hmº) de adutos por termogravimetria Artigo

    Farias, Robson Fernandes de

    Resumo em Inglês:

    An empirical equation: deltaD HmO = t i/2.2(2-n) is obtained and tested for 102 adducts (mainly adducts with zinc group halides). In the equation, t i is the Kelvin temperature of the beginning of the thermal decomposition of the adduct, (obtained by thermogravimetry), and n is the number of ligands. For 1/3 of the tested adducts the difference between experimental and calculated values was less than 5%. For about 1/3 of the adducts that difference exceeds 15%.
  • Os DNA sintéticos anti-sentido Revisão

    Cravador, Alfredo

    Resumo em Inglês:

    One old dream of the chemist in the field of the drug research is to create molecules capable of reaching their target with the precision of a missile. To accomplish it these molecules must have the propriety of distinguishing qualitative differences between healthy and diseased cells. A therapy based on this principle, able of eradicating specifically defective cells, or cells affected by a pathogen has an enormous advantage with the regard to the classical approach in which the cytotoxic drugs merely exploit quantitative biochemical and kinetic differences between abnormal and normal cells. We present in this article a review on the chemical synthesis of analogues of desoxyribonucleotides and on results obtained on the specific and irreversible inhibition of undesired genetic expression using the antisense principle.
  • Íons nitrênio Revisão

    Mota, Claudio J. A.

    Resumo em Inglês:

    This paper reviews the chemistry of nitrenium ions, the nitrogen analogues of the carbenium ions, showing the pioneering studies and some synthetic applications.
  • Amostragem de suspensões: Emprego da técnica na análise direta de amostras Revisão

    Magalhães, Carlos Emanuel de Carvalho; Arruda, Marco Aurélio Zezzi

    Resumo em Inglês:

    This review presents some characteristics related to slurry sampling in trace analysis in terms of its advantages, limitations and applications, as well as the latest advance in this area, such as mechanization, chemical modifiers, stabilization agents and others. The reviewed applications include foods, biological and geological materials.
  • Uma introdução à análise exploratória de dados multivariados Divulgação

    Moita Neto, José Machado; Moita, Graziella Ciaramella

    Resumo em Inglês:

    The modern technological ability to handle large amounts of information confronts the chemist with the necessity to re-evaluate the statistical tools he routinely uses. Multivariate statistics furnishes theoretical bases for analyzing systems involving large numbers of variables. The mathematical calculations required for these systems are no longer an obstacle due to the existence of statistical packages that furnish multivariate analysis options. Here basic concepts of two multivariate statistical techniques, principal component and hierarchical cluster analysis that have received broad acceptance for treating chemical data are discussed.
  • Sistemas transportadores de drogas Divulgação

    Montanari, Maria Luiza C.; Montanari, Carlos Alberto; Piló-Veloso, Dorila; Beezer, A. E.; Mitchell, J. C.

    Resumo em Inglês:

    Drug delivery system controls the distribution of drugs for optimal therapeutic efficacy. The complex of higly active drugs with macromolecular carriers seems to offer a promising way to optimize their delivery. Dendrimers can be used as drug delivery system and this paper addresses the effectivenes of the approach. The host-guest system improves the solubility of hydrazides and mesoionic 1,3,4-thiadiazolium-2-aminide compounds.
  • Eletrodos artesanais para voltametria Nota Técnica

    Silva, Reinaldo Carvalho; Souza, Ivan Gonçalves de

    Resumo em Inglês:

    This paper describes the construction and performance of homemade electrodes for voltammetric purpose using cheap materials, like pipette tips and asbestos fiber. A good cost-to-benefit relation makes this devices specially designed for student use, expecting to improve the broadcasting of electroanalytical methods in Brazilian schools.
  • Determinação de traços de Co e Co2 "em linha" por cromatografia em fase gasosa Nota Técnica

    Jesus, Rosangela Novaes de; Andrade, Jailson B. de

    Resumo em Inglês:

    The present work describes a rapid and sensitive method for the determination of carbon monoxide and carbon dioxide at low concentration levels, on line, in ethylene and hydrogen lines. These gases were separated in a column filled with Porapak Q, converted to methane and quantified by a flame ionization detector. Some modifications were made in the injection system and in the lines of the carrier gas. The detection limits of 2,6 ppbV and 4,85 ppbV for CO and CO2, respectively, were reached after modifications.
  • Nova rota de preparação do 2-cloro-1,3,2-dioxofosfolana e 2-cloro-4,5-benzo-1,3,2-dioxofosfolana e caracterização por espectroscopia de RMN multinuclear Nota Técnica

    Costa, Ricardo França Furtado da; Passos, Bernadette de F. Trigo; Matos, Robson Mendes

    Resumo em Inglês:

    A new method for the preparation of 2-chloro-1,3,2-dioxaphospholane (1) and 2-chloro-4,5-benzo-1,3,2-dioxaphospholane (2), are reported. The modifications introduced in the synthetic route improved the yield and facilitated the control of reaction, but the synthesis require longer reaction time. The compounds were characterized by ¹H, 13C{¹H} and31P{¹H} NMR spectroscopy. Due to the complexity of the spin system AA'BB'X (A, A', B, B' = ¹H; X = 31P) of 2, a simulation of the ¹H NMR spectra was done and it's in agreement with the bibliography.
  • Interfase y software de control para operar en sincronismo un automuestreador y un atomizador electrotérmico por filamento de tungsteno en espectrofotometría de absorción atómica

    Neira, J.; Valenzuela, G.; Vega, J.; Moya, J.; Bruhn, C. G.; Nóbrega, J. A.

    Resumo em Inglês:

    The interface and software for synchronous control of an autosampler and an electrothermal tungsten coil atomizer in atomic absorption spectrophotometry were developed. The control of the power supply, the trigger of the Read function of the spectrophotometer and the automatic operation of the autosampler was performed by software written in "TurboBasic". The system was evaluated by comparison of the repeatability of peak-height absorbances obtained in the atomization of lead by consecutive 10-µl injections of solutions (prepared in 0.2% v/v HNO3) using autosampler and manual sample introduction, and also by long term operation.
  • Potencialidades do dióxido de chumbo eletrodepositado como sensor potenciométrico Educação

    Capelato, Milton Duffles; Cassiano, Neila Maria

    Resumo em Inglês:

    This paper proposes an experiment to be performed in both instrumental analysis and experimental physical-chemistry curricular disciplines in order to open options to develop challenging basic research activities. Thus the experimental procedures and the results obtained in the preparation of electrodeposited lead dioxide onto graphite and its evaluation as potentiometric sensor for H3O+ and Pb2+ ions, are presented. The data obtained in acid-base titrations were compared with those of the traditional combination glass electrode at the same conditions. Although a linear sub-Nernstian response to free hydrogen ions was observed for the electrodeposited PbO2 electrode, a good agreement was obtained between them. Working as lead(II) sensing electrode, the PbO2 showed a linear sub-Nernstian behavior at total Pb2+ concentrations ranging from 3,5 x 10-4 to 3,0 x 10-2 mol/L in nitrate media. For the redox couple PbO2/Pb(II) the operational slope converges to the theoretical one, as the acidity of the working solution increases.
  • A formulação ab-initio da segunda lei da termodinâmica Educação

    Braga, J. P.

    Resumo em Inglês:

    This paper deals with Carathédory's formulation of the second law of thermodynamics. The material is presented in a didatical way, which allows a second year undergraduate student to follow the formalism. An application is made to an ideal gas with two independent variables. A criticism to Carnot formulation of the second law and an investigation of the historical origins of the Carathéodory formalism are also presented.
  • Algumas considerações sobre as origens da preparação de ácido nítrico Assuntos Gerais

    Beltran, Maria Helena Roxo

    Resumo em Inglês:

    It is commonly acknowledged that the earliest recipe to prepare mineral acids dates from the XIIIth century, since it can be found in a text attributed to Geber. This paper intends to discuss this belief, taking into account recent studies on the Geberian corpus and also considering some ancient references to saltpeter.
  • Vidros recobertos com camadas delgadas transparentes de SnO2 Assuntos Gerais

    Rizzato, Alessandro P.; Pulcinelli, Sandra H.; Santilli, Celso V.

    Resumo em Inglês:

    SnO2 thin layers, prepared from aqueous colloidal suspensions by the sol-gel process, have been dip-coated on commercial borosilicate glasses. The effect of the conditions of deposition on the optical and structural characteristics of the thin layers was analysed by UV-Vis spectroscopy, x-ray reflectometry and electron scanning microscopy. Layers prepared with withdrawal speed in between 0.1 and 10cm/min show thickness smaller than 90nm, roughness of the order of 2nm and transmittance higher than 80%, resulting in good optical quality samples. The roughness increases from 2 to 11nm as the withdrawal speed increases from 10 to 80cm/min, what seems to be associated to the enlargement of the layers thickness (> 90nm). The measurements of mass loss, done after etching with fluoridric acid show that the coated samples are more corrosion resistant than the uncoated borosilicate glass.
  • Connectivity in sol-gel silica glasses

    Vasconcelos, Wander L.

    Resumo em Inglês:

    In this work it is carried out a review on structural parameters related to the evaluation of pore connectivity of nanostructures. The work describes parameters and methods of evaluation of geometric parameters. The concepts of connectivity are applied to silica gels and glasses obtained from sol-gel process. The study of pores connectivity was carried out using a combination of geometric modeling and experimental evaluation of specific surface area and pore volume. The permeability of the pore structure is evaluated and a permeability geometric factor, Pg, is proposed.
  • Estudo das propriedades ópticas em vidros 0,3La2S3-0,7Ga2S 3 Assuntos Gerais

    Marmolejo, Edgar M.; Paula, Ana M. de; Reynoso, V. C. S.; Barbosa, Luiz C.; Alves, Oswaldo L.

    Resumo em Inglês:

    In this work we describe the synthesis and characterization of chalcogenide glass (0.3La2S3-0.7Ga2S 3) with low phonons frequencies. Several properties were measured like Sellmeier parameters, linear refractive index dispersion and material dispersion. Samples with the composition above were doped with Dy2S3. The absorption and emission characteristics were measured by electronic spectroscopy and fluorescence spectrum respectively. Raman and infrared spectroscopy shows that these glasses present low phonons frequencies and strucuture composed by GaS4 tetrahedrals. The Lines model was used for calculate the coefficients values of the non linear refractive index.
  • Espectroscopia óptica de vidros fluoroindatos dopados com íons Er3+ e Yb3+ Assuntos Gerais

    Ribeiro, C. T. M.; Zanatta, A. R.; Sartori, J.; Nunes, L. A. O.; Messaddeq, Y.

    Resumo em Inglês:

    Optical spectroscopy in the 400-1700nm wavelength range was performed on rare earth doped heavy metal fluoride (HMF) glasses. In the present work In-based fluoride glasses with a fixed 2 mol % YbF3 concentration and an ErF3 content ranging from 0 to 8 mol % were investigated. According to the experimental spectroscopic data a dependence in the absorption coefficient, the photoluminescence intensity and in the radiative lifetime could be verified as a function of the ErF3 content. In addition, at liquid nitrogen temperature, light emission corresponding to indirect transitions in the infrared energy range could be easily observed as a consequence of the low phonon frequency characteristic of this class of fluoride glasses. For all the studied compositions, strong upconversion to the green and red light was observed by pumping these Er3+- and Yb3+-doped HMF glasses with 790 and 980nm photon sources.
  • Influência da adição de defloculante, ligante e partículas de alumina no comportamento reológico de suspensões a base de frita e caulim Assuntos Gerais

    Hotza, Dachamir; Fredel, Márcio C.; Rodrigues Neto, João B.; Alarcon, Orestes E.

    Resumo em Inglês:

    Enamel suspensions were characterized according to their rheological behavior. The suspensions presented a pseudoplastic behavior, yield stress and thixotropy, with or without the presence of deffloculant. Added carboxymethylcellulose increases the apparent viscosity of enamel suspensions and interacts complexly with the deffloculant, here sodium silicate. Addition of crystalline particles of two types of alumina, used to improve the wear resistance of ceramic glazes, also change strongly the rheological behavior of the suspensions. Added high specific area, irregular alumina particles produce a higher increase of the apparent viscosity of enamel suspensions compared to rounded ones.
  • Ostwald ripening in porous materials

    Schmelzer, Jürn; Möller, Jörg; Slezov, Vitali V.; Gutzow, Iwan; Pascova, R.

    Resumo em Inglês:

    The process of coarsening of an ensemble of clusters is investigated for the case that elastic strains due to matrix - cluster interactions change the process qualitatively as compared with dependencies established theoretically first by Lifshitz and Slezov. Such a qualitatively different behavior occurs always when the energy of elastic deformation in cluster growth increases more rapidly than linear with the volume of a cluster. Analytic solutions, for limiting cases, as well as numerical solutions, for the general case of coarsening in an ensemble of pores with a given pore size distribution, are presented. Possible applications are discussed.
  • Efeito da adição de Na2O na viscosidade e devitrificação do vidro obtido a partir de cinzas volantes e Li2O Assuntos Gerais

    Neves, Etney; Poffo, Edoardo D.; Fredel, Márcio C.; Riella, Humberto G.; Alarcon, Orestes E.

    Resumo em Inglês:

    Glass-ceramic materials can be produced by the addition of LiO2 to fly ashes disposible in Southern Brazil. These glass-ceramics are based on the Al2O3-SiO2-Li 2O system. The high viscosity of the obtained glasses, however, makes forming useful articles with these materials difficult. In this study we investigate the effect of adding low cost Na2CO3 on the melt viscosity and on the nature of the developed crystalline phases. It was intended that the ultimate crystalline phase (LiAlSi3O8) should not be altered. With additions up to 3 wt. % Na2CO3, the viscosity was apparently lowered and no new crystalline phase were detected.
  • Carta ao editor Assuntos Gerais

    Berlinck, Roberto G. S.
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