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Química Nova, Volume: 21, Número: 5, Publicado: 1998
  • Editorial

    Alves, Oswaldo L.; Barreiro, Eliezer J.
  • Estudo do comportamento ácido-base da 4,4'-ditiodipiridina Artigo

    Moreira, Ícaro de Sousa; Parente, Letícia Tarquinio de Sousa; Franco, Douglas Wagner

    Resumo em Inglês:

    Despite the importance of the 4,4'-dithiodipyridine as an electrode modifier on the protein electrochemical studies and as a remarkable bridged-ligand on conducting electronic density in binuclear mixed valence complexes, there is no data available in the literature concerning acid-base behavior of this compound. Aiming to afford such information we undertook the ionization equilibrium study of this ligand. Although two acid species, DTDPH+ and DTDPH2+ have been detected in solution, only the diacid-form was possible to be isolated as a perclorate salt DTDPH2(ClO4)2. The ionization constants for the two step equilibrium processes (pKa1=2.70 and pKa2=4.80) were determined by using the spectrophotometric technique and aqueous solutions of CF3COONa, mu=0,1 mol.L-1 .
  • Metais pesados em águas superficiais como estratégia de caracterização de bacias hidrográficas Artigo

    Yabe, Maria Josefa Santos; Oliveira, Elisabeth de

    Resumo em Inglês:

    The input of heavy metals concentrations determinated by ICP-AES, in samples of the Cambé river basin, was evaluated by using the Principal Component Analysis. The results distinguishes clearly one site, which is strongly influenced by almost all elements studied. Special attention was given to Pb, because of the presence of one battery industry in this area. Some downstream samples were associated with the same characteristics of this site, showing residual action of contaminants along the basin. Other sites presented influence of soil elements, plus Cr near a tannery industry. This study allowed to distinguish different sites in the upper basin of the Cambé (Londrina-PR-BR), in accordance to elements input.
  • Estudo fitoquímico de Unonopsis lindmanii - Annonaceae, biomonitorado pelo ensaio de toxicidade sobre a Artemia salina leach Artigo

    Siqueira, João Máximo de; Bomm, Mauro Dionei; Pereira, Núbia Fernanda Gomes; Garcez, Walmir Silva; Boaventura, Maria Amélia Diamantino

    Resumo em Inglês:

    Extracts obtained from leaves, seeds and bark of Unonopsis lindmanii were evaluated by means of Brine Shrimp Lethality test (BSL). Through bioassay-guided chromatographic fractionation, liriodenine, an oxoaporphine alkaloid, was isolated from the bark extracts as the bioactive compound. Two additional inactive known alkaloids, unonopsine and lysicamine were also isolated from the bark extracts.
  • Decomposição catalítica de óleo de soja em presença de diferentes zeólitas Artigo

    Santos, Frances R.; Ferreira, José Carlos Netto; Costa, Stella R. Reis da

    Resumo em Inglês:

    The catalytic decomposition of soybean oil was studied in a fix bed reactor at 673 and 773 K and using amorphous silica-alumina and the zeolites USY, H-Mordenite and H-ZSM-5 as catalysts. Both the selectivity and the catalytic activity were determined by studying the product composition resulting from the chemical reactions. Physicochemical characteristics of the catalysts were obtained by X-ray fluorescence, Fourier Transform infrared spectroscopy, 29Si and 27Al Nuclear Magnetic Ressonance and textural analysis. The zeolites USY and H-ZSM-5, showing higher Brönsted acidity, yielded products with higher concentration in aromatic hydrocarbons, whereas with both H-Mordenite and amorphous silica-alumina the main products were paraffins.
  • Síntese e caracterização de cloro[ácido 2-(difenilfosfino)benzóico]-ouro(I) e alguns de seus derivados Artigo

    Howe, B. P.; Parish, R. V.; Pritchard, R. G.

    Resumo em Inglês:

    In this contribution a few new gold(I)phosphine complexes, [2-(PPh2)C6H4CO 2H]AuX (where X = Cl, SCN, Br3) and a similar gold(III) derivative [{2-(PPh2)C6H4CO 2H}AuIII Cl (C6H4CH2NMe2 )]Cl have been synthesised and characterised. The phosphine, 2-(diphenylphosphino)benzoic acid, has been employed for the first time in gold chemistry. This ligand is potentially bidentate through bonding of the phosphine and carboxylate groups. The X-ray structure of the complex chloro[2-(diphenylphosphino) benzoic acid]gold(I) has been elucidated and the bond lengths encountered show great similarity to those of chloro(triphenylphosphine)gold(I). [2-(PPh2)C6H4CO 2H]AuCl crystallises in the space group P2(1)/c with a = 9.113(2) Å, b = 10.925(2) Å, c = 23.069(4) Å, beta = 99.95º(3), V = 2299 ų, Z = 4 and R = 0.091. Biological tests for anti-fungal and anti-bacterial activity demostrate that [2-(PPh2)C6H4CO 2H]AuCl exhibits broad spectrum activity against a range of organisms.
  • Isolamento e caracterização de acil-tiossemicarbazidas como intermediários na síntese de compostos mesoiônicos Artigo

    Maciel, M. A. M.; Echevarria, A.; Rumjanek, V. M.

    Resumo em Inglês:

    1,3,4-thiadiazolium-2-aminides and their isomers 1,3,4-triazolium-2-thiolates have been synthesized via anhydroacylation reactions. This work presents a study by infrared monitoring of the reaction between substituted aroyl acid chlorides and 1,4-diphenylthiosemcarbazide. The intermediates and products were isolated, purified and charaterized by IR and 13C NMR spectroscopy. The increasing or decreasing in intensity of characteristic stretching bands indicated the rate dependence on the electronic nature of substituents. The results also demonstrate that 1,3,4-triazolium-2-thiolates are obtained in anhydrous conditions whereas presence of water leads to a mixture of the isomers.
  • Síntese e atividade antibacteriana de imidas cíclicas: 3,4-dicloromaleimidas e 3-cloro-4-substituída-maleimidas Artigo

    Andricopulo, Adriano Defini; Yunes, Rosendo Augusto; Nunes, Ricardo José; Savi, Alessandro O. S.; Corrêa, Rogério; Cruz, Alexandre Bella; Cechinel Filho, Valdir

    Resumo em Inglês:

    In the present study, new N-aryl and N-alkylarylcyclic imides were synthesized and their antibacterial properties against Escherichia coli and Staphylococcus aureus were evaluated by using the diffusion method. All compounds were obtained in good yield (54 - 95%) and characterized by spectral data (¹H-NMR, MS, IR) and elemental analysis (CHN). The biological results indicated that some compounds exert significative antibacterial effects, confirming previous studies on biological activities of cyclic imides.
  • Ozonólise das ligninas organossolve e kraft eucalipto. Parte II: cinética nos meios ácido e básico Artigo

    Nascimento, Evandro A.; Morais, Sérgio A. L.; Aquino, Francisco J. T.; Piló - Veloso, Dorila

    Resumo em Inglês:

    Organosolv and kraft lignins were treated with ozone both in basic and acid media and the reaction was studied kinetically. In contrast to reported studies, ozone was more efective in basic medium. Kraft lignin was degraded faster than organosolv lignin in both media but in the basic medium the rate of reaction was very much faster than in the acid one: for kraft lignin, the observed degradation was 93% for 2 min of reaction in the basic medium and 56% for 10 min of reaction in the acid medium; for organosolv lignin, 47% and 25%, respectively, in the same times. Higher phenolic hydroxyl groups contents increase the reaction rate.
  • Determinação de fósforo orgânico em águas de produção petrolífera por ICP- AES e ICP- MS após pré-concentração em coluna de sílica-C18 Artigo

    Rocha, Anderson Araújo; Miekeley, Norbert; Silveira, Carmem Lúcia Porto da; Bezerra, Maria Carmem Moreira

    Resumo em Inglês:

    Results on the optimization of analytical methods for the determination of phosphorus in phosphino-polycarboxylate (PPCA), used frequently as scale inhibitor during oil production, by ICP-AES and ICP-MS are presented. Due to the complex matrix of production waters (brines) and their high concentration in inorganic phosphorus, the separation of organic phosphorus prior to its determination is necessary. In this work, minicolumns of silica immobilized C18 were used. Optimization of the separation step resulted in the following working conditions: (1) prewashing of the column with methanol (80% v/v); (2) use of a flow rate of 5 mL/min and 10 mL/min, respectively, for the preconditioning step and for percolation of the water sample; (3) final elution of organic phosphorus with 7 mL of buffer of H3BO3/NaOH (0.05 M, pH 9) with a flow rate of 1 mL/min. Sample detection limits (3s) for different combinations of nebulizers and spectrometric methods, based on 10 mL water aliquots, are: ICP-AES -Cross flow (47 mg/L) and Ultrasonic (18 mug/L); ICP-MS -Cross flow (1.2 mug/L), Cyclonic (0.7 mug/L) and Ultrasonic (0.5 mug/L). Typical recoveries of organic phosphorus are between 90 and 95% and the repeatability of the whole procedure is better than 10%. The developed methodology was applied successfully to samples from the oil-well NA 46, platform PNA 2, Campos basin, Brazil. Assessment of the PPCA inhibitor was possible at lower concentrations than achieved by current analytical methods, resulting in benefits such as reduced cost of chemicals, postponed oil production and lower environmental impacts.
  • Calibração multivariada para sistemas com bandas sobrepostas através da análise da fatores do tipo Q Artigo

    Scarminio, Ieda Spacino; Ishikawa, Dilson Norio; Barreto, Wagner José; Paczkowski, Édio Luiz; Arruda, Iara Cintra

    Resumo em Inglês:

    A multivariate calibration method to determine chemical compositions of systems with severely overlapped bands is proposed. Q mode factors are determined from the spectral data and subsequently rotated using the varimax and oblique transformation of Imbrie. The method is applied to two sets of simulated data to test the sensitivity of analytical results to random experimental error. The chemical concentrations of alanine and threonine mixture are determined from spectral data of the 302,5 - 548,5 nm region.
  • Estratégias sintéticas para o ácido nonático Revisão

    Ferraz, Helena M. C.; Payret-Arrúa, M. Elena

    Resumo em Inglês:

    Nonactic Acid is the monomeric unity of the Nactines, an important class of poliether antibiotics. This review focuses on the approaches to the syntheses of the above mentioned unity, which have been accomplished in the period from 1971 to date.
  • Rotas de síntese e a homogeneidade dos precursores de mulita e cordierita Revisão

    Lima, Patrícia Tavares de; Bertran, Celso Aparecido; Thim, Gilmar Patrocínio

    Resumo em Inglês:

    Multicomponent ceramics are mainly synthesized by conventional solid-state reaction route and sol-gel routes. In the sol-gel route, colloidal or polymeric gel are envolved. In this work, some principles of the chemistry of theses routes are discused and it is ilustrated a variety of strategies for obtaining a homogeneous multicomponent precursors.
  • Eletrodos fabricados por "silk-screen" Revisão

    Nascimento, Valberes B.; Angnes, Lúcio

    Resumo em Inglês:

    A review dealing with the use of screen-printing technology to manufacture disposable electrodes is presented, covering in details virtually all the publications in the area up to early 1997 and including 206 references. The elements and different strategies on constructing modified electrodes are highlighted. Commercial and Home-made ink recipes are discussed. Microelectrode arrays, built by the combination of photostructuring and screen-printing technologies to the mass production of advanced disposable sensors, are also discussed. Future research trends are predicted.
  • Agentes complexantes: podante, coronante e criptante classificação e nomenclatura Divulgação

    Whei, Oh Lin; Brito Neto, José Thomé Xavier de

    Resumo em Inglês:

    The scientific and practical interest in crown ethers as complexing agents for actions as well as for anions and neutral low molecular species is undeniable. New molecules with crown ether properties are constantly synthesized and new application discovered. This paper presents classification and nomenclature of the classical oligoethers (crown ethers): monocyclic coronands; oligocyclic spherical cryptands; and acyclic podands.
  • O uso de calorimetria em ecologia Divulgação

    Airoldi, Claudio

    Resumo em Inglês:

    The macroscopic effects caused by sun radiation and the mankind-nature interactions in a ecosystem are firstly presented. However, the importance of calorimetric determinations to clarify some phenomena related to the living microorganism populations and their interactions with the food additive or inhibitor agents are reported. The collect values illustrate the occurence a great deal of effects in this microscopic world. For this subject, the reachest Latosol soil was selected due to the content of organic matter and consequently in microorganisms. Microbial activity was stimulated by addition of glucose, which showed to be the best nutrient source. Inhibitory effect was detected with many compounds used in the agriculture like some herbicides and fungicides. Although the assays are based on the use of the microcalorimetry, other techniques like respirometry contributes strongly to the understanding of the ecosystem. The main objective in this exposition is to stimulate by means of many interesting examples, the importance of preserving the environment in order to establish direct analogies by using the Chemistry in the daily life.
  • Ácido L-ascórbico: reações de complexação e de óxido-redução com alguns íons metálicos de transição Divulgação

    Fornaro, Adalgiza; Coichev, Nina

    Resumo em Inglês:

    The strong reducing action of L-ascorbic acid (Vitamin C) are of fundamental interest in biochemical and related process. The oxidation of ascorbic acid by molecular oxygen and others oxidants are of fundamental importance, involving the intervention of transition metal ions as catalysts and the formation transition metal complexes of ascorbic acid as intermediates. The present article is intended to cover some aspects of the reactions of ascorbic acid and related compounds involving some transition metal ions.
  • Determinação de potássio em méis após precipitação com tetrafenilborato de sódio e separação em coluna de troca-iônica Nota Técnica

    Azeredo, Maria Aparecida Alves; Azeredo, Laerte da Cunha; Soares, Jucelane de Castro Alcântara

    Resumo em Inglês:

    A new method for determination of potassium in honey samples of different colors was developed as an alternative method for determination of this metal. Analysis of genuine honeys attested by the qualities and quantities tests officially adopted in Brazil, showed that the concentration of potassium ranged from 181 to 315 mg/kg for light honeys, from 393 to 570 mg/kg for medium honeys and from 791 to 915 mg/kg for dark honeys. Recoveries making use of spikes of potassium added to the honey samples and to the deionized distilled water showed results close by hundred percent at pH <= 2,0 under temperature bellow 20°C.
  • Utilização de uma interface do tipo "particle beam" para a obtenção de espectros de massas de compostos pouco voláteis em solução Nota Técnica

    Augusti, Rodinei; Dias, Adelson de O.; Fortes, Isabel C. P.

    Resumo em Inglês:

    Due to source contamination and wearing of instrument components problems caused by the direct insertion probe technique, a new way of introduction of low volatile compounds into mass spectrometer was tested. This new scheme comprises the introduction of the low volatile compounds solutions via a six port valve connected to a particle beam interface. Solutions of isatin were injected into this system and the best results were obtained with CH2Cl2, CH3OH and CH3CN. The solution inlet system has shown to be advantageous over the conventional way of direct insertion probe introduction.
  • Automatização de um destilador d'água Nota Técnica

    Neves, Carlos A.; Gutz, Ivano G. R.; Lago, Claudimir L. do

    Resumo em Inglês:

    A simple and inexpensive device to automate a water distilling apparatus is shown. It is composed by a magnetic floater placed in the water reservoir and a level control unit, which acts over the heating element circuit. In order to provide water saving, an electromagnetic valve is inserted in the water supply inlet. Some suggestions for the adaptation to other types of equipment are also offered.
  • Determinação permanganimétrica de íons Fe3+ com o uso de zinco metálico como redutor - uma contribuição ao ensino de química analítica Educação

    Lichtig, Jaim; Rocha, Marcos; Táboas, Regina G. Z.; Röpke, Sacha

    Resumo em Inglês:

    The classical volumetric titration of Fe2+ with MnO4-, used in some routine analysis as well as in undergraduate courses was improved. SnCl2 (to reduce Fe3+ to Fe2+) and HgCl2 (to oxidize excess SnCl2) were substituted by metallic zinc in boiling solutions, thus avoiding the toxic HgCl2 and Hg2Cl2; nitrate ions do not interfere in the improved methodology (it is an interference in the classical one) and the reproducibility of the determinations is increased by using metallic zinc. Determinations by students of undergraduate courses are discussed.
  • Modelos para o carbono sp³: quatro pirâmides no tetraedro Educação

    Constantino, Mauricio Gomes; Souza, Altamiro Xavier de

    Resumo em Inglês:

    We describe a paper model for the sp³ carbon atom, consisting of four pyramids that can be assembled to produce a tetrahedron. The main feature of this model is that, when two of the pyramids are properly put together, the solid thus formed is an "open" tetrahedron, containing edges connecting the center of the tetrahedron to its vertices. The student can easily imagine the whole tetrahedron and, at the same time, he can observe its center and the lines corresponding to the directions of sp³ orbitals.
  • Theodoro Peckolt: naturalista e farmacêutico do Brasil Imperial Assuntos Gerais

    Santos, Nadja Paraense dos; Pinto, Angelo C.; Alencastro, Ricardo Bicca de

    Resumo em Inglês:

    In this paper we briefly describe the scientific career of Theodor Peckolt, naturalist and pharmacist, and his seminal contribution to the development of phytochemistry in Brazil. His achievements are discussed in the light of the historical background of the Brazilian science and University at his time.
  • Gerenciamento de resíduos químicos em laboratórios de ensino e pesquisa Assuntos Gerais

    Jardim, Wilson de Figueiredo

    Resumo em Inglês:

    The generation of chemical residues in both teaching and research laboratories is a serious problem in Brazil. In this article, a Chemical Residues Management Program is presented and discussed. The Program is centered in different hierarchic positions, but driven by minimization. A common ground for discussion and distribution of related information is also proposed as a mean to spread the program throughout Brazilian Universities.
  • Carta ao editor Assuntos Gerais

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