Síntese, caracterização, propriedades e aplicação dos sistemas Mg- Al, Zn-Al e Mg-Fe

The Layered Double Hydroxides has become extremely promising materials due to its range of applications, easily obtained in the laboratory and reusability after calcination, so the knowledge regarding their properties is of utmost importance. In this study were synthesized layered double hydroxides of two systems, Mg-Al and Zn-Al, and such materials were analyzed with X-ray diffraction and, from these data, we determined the volume density, planar atomic density, size crystallite, lattice parameters, interplanar spacing and interlayer space available. Such materials were also subjected to thermogravimetric analysis reasons for heating 5, 10, 20 and 25 ° C / min to determine kinetic parameters for the formation of metaphases HTD and HTB based on theoretical models Ozawa, Flynn-Wall Starink and Model Free Kinetics. In addition, the layered double hydroxides synthesized in this working ratios were calcined heating 2.5 ° C / min and 20 ° C / min, and tested for adsorption of nitrate anion in aqueous solution batch system at time intervals 5 min, 15 min, 30 min, 1h, 2h and 4h. Such calcined materials were also subjected to exposure to the atmosphere and at intervals of 1 week, 2 weeks and 1 month were analyzed by infrared spectroscopy to study the kinetics of regeneration determining structural called "memory effect"

Síntese hidrotérmica e caracterização estrutural de titanatos nanotubulares para aplicação na captura do dióxido de carbono

Nanostructured materials have been spreading successfully over past years due its size and unusual properties, resulting in an exponential growth of research activities devoted to nanoscience and nanotechnology, which has stimulated the search for different methods to control main properties of nanomaterials and make them suitable for applications with high added value. In the late 90 s an alternative and low cost method was proposed from alkaline hydrothermal synthesis of nanotubes. Based on this context, the objective of this work was to prepare different materials based on TiO2 anatase using hydrothermal synthesis method proposed by Kasuga and submit them to an acid wash treatment, in order to check the structural behavior of final samples. They were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), adsorption/desorption of N2, thermal analysis (TG/DTA) and various spectroscopic methods such as absorption spectroscopy in the infrared (FT-IR), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). All the information of characterizations confirmed the complete conversion of anatase TiO2 in nanotubes titanates (TTNT). Observing the influence of acid washing treatment in titanates structure, it was concluded that the nanotubes are formed during heat treatment, the sample which was not subjected to this process also achieved a complete phase transformation, as showed in crystallography and morphology results, however the surface area of them practically doubled after the acid washing. By spectroscopy was performed a discussion about chemical composition of these titanates, obtaining relevant results. Finally, it was observed that the products obtained in this work are potential materials for various applications in adsorption, catalysis and photocatalysis, showing great promise in CO2 capture

Aplicação das técnicas eletroanalíticas (voltametria cíclica e de pulso diferencial) usando o eletrodo de diamante dopado com boro para o estudo da isoniazida, etambutol, rifampicina e pirazinamida

In this work a study was done using electrochemical cyclic voltammetry and differential pulse voltammetry for isoniazida (INH), ethambutol (EMB), rifampicina (RIF) and pyrazinamide (PZA) using the electrode boron-doped diamond (BDD) as working electrode. It also verified the applicability of the technique of differential pulse voltammetry in the quantification of the active compounds used in the treatment of tuberculosis, subsequently applying in samples of pharmaceutical formulation. Among the four active compounds studied, isoniazid showed the best results for the detection and quantification using differential pulse voltammetry. At pH 4 and pH 8, for the calibration curves to INH showed good linearity, with quantification limits of 6.15 mmol L-1 (0,844 ppm) and 4.08 mmol L-1 (0.560 ppm) for the respective pH. The proposed method can be used to determine drug isoniazid, for recovery values were obtained in approximately 100%

Recuperação de um solo degradado com a aplicação de adubos verdes e lodo de esgoto

A utilização incorreta dos solos vem causando alterações neles, tornando-os cada vez menos produtivos, aumentando as áreas com solos degradados. O presente trabalho teve por objetivos estudar ações para acelerar a formação do horizonte A de um Latossolo Vermelho degradado, via uso de adubos verdes, lodo de esgoto e cultivo de uma espécie arbórea nativa de Cerrado, e selecionar indicadores para detectar alterações da camada superficial do solo. O monitoramento das alterações do solo foi realizado anualmente. O delineamento experimental foi o de blocos casualizados com seis tratamentos, em cinco repetições. Os tratamentos foram: testemunha - solo exposto (sem manejo); vegetação nativa (Cerrado); espécie arbórea Astronium fraxinifolium; Astronium fraxinifolium + Canavalia ensiformis; Astronium fraxinifolium + Raphanus sativus; e Astronium fraxinifolium + Brachiaria decumbens + lodo de esgoto (60 t ha-1). Avaliou-se no solo: porosidade, densidade do solo, cátions trocáveis, pH, acidez potencial (H + Al), soma de bases (SB), saturação por bases (V), CTC e macrorganismos. Nos adubos verdes, foi avaliada a massa seca e, para a espécie arbórea, a altura e o diâmetro de caule. A mobilização do solo e a mobilização mais a adubação verde e o lodo de esgoto estão recuperando as propriedades do solo degradado, com comportamento semelhante entre elas após um ano de adoção. O melhor indicador físico das alterações do solo foi sua densidade. Os tratamentos adotados são semelhantes quanto à população de macrorganismos do solo e contribuindo positivamente para recuperação da macrofauna. A presença de larva e besouro foi indicadora da melhoria da macrofauna do solo.

Atributos físico-hídricos de um Latossolo após a aplicação de lodo de esgoto em área degradada do Cerrado

Os solos cultivados intensivamente e inadequadamente são degradados, assim como a construção de obras civis no meio rural executada sem atender à legislação. O trabalho objetivou definir a interferência do lodo de esgoto na recuperação de atributos de um Latossolo Vermelho. O experimento foi implantado em 2004, em Selviria (MS). Os tratamentos utilizados foram: T1-vegetação de cerrado; T2-solo exposto sem tratamento para recuperação; T3-solo cultivado com eucalipto e braquiária sem o uso do lodo de esgoto e adubação mineral; T4-solo cultivado com eucalipto e braquiária com adubação mineral; T5-solo cultivado com eucalipto e braquiária com uso de 30Mg ha-1 de lodo de esgoto e; T6-solo cultivado com eucalipto e braquiária com uso de 60Mg ha-1 de lodo de esgoto. Nas camadas do solo de 0,00-0,05; 0,05-0,10; 0,10-0,20 e de 0,20-0,30m, foram avaliados os atributos físico-hídricos e teor de matéria orgânica. Os tratamentos com adubação mineral e orgânica estão agindo de forma semelhante para a recuperação dos atributos físico-hídricos e do teor de matéria orgânica. em solos degradados pela construção de obras civis a aplicação de 30 a 60mg de lodo de esgoto ha-1 recupera as suas propriedades físico-hídricas.

Aplicação da termogravimetria na determinação do teor de ferro em comprimidos: um estudo comparativo com a espectrofotometria

This study used the Thermogravimetry (TG) and molecular absorption spectroscopy in UV-visible region to determine the iron content in herbal medicinal ferrous sulfate used in the treatment of iron deficiency anemia. The samples were characterized by IR, UV, TG / DTG, DTA, DSC and XRD. The thermoanalytical techniques evaluated the thermal stability and physicochemical events and showed that the excipients interfere in the decomposition of the active ingredients. The results of thermogravimetry showed that the decomposition temperature of the active principle Fe2(SO4)3 (T = 602 °C) is higher as compared to samples of tablets (566 586 °C). In the DTA and DSC curves were observed exothermic and endo events for samples of medicines and active analysis. The infrared spectra identified key functional groups exist in all samples of active ingredients, excipients and compressed studied, such as symmetric and asymmetric stretching of OH, CH, S=O. The analysis by X-ray diffraction showed that all samples had crystallinity and the final residue showed peaks indicating the presence of silicon dioxide, titanium dioxide and talc that are excipients contained in pharmaceutical formulations in addition to iron oxide. The results obtained by TG to determine the iron content of the studied drugs showed a variance when compared with those obtained by theoretical and UV-visible, probably due to formation of a mixture of Fe2O3 and Fe2(SO4)3. In one tablet was obtained FE content of 15.7 % and 20.6 % for TG by UV-visible, the sample EF 2 was obtained as a percentage of 15.4 % and 21.0 % for TG by UV-visible . In the third SF samples were obtained a content of 16.1 % and 25.5 % in TG by UV-visible, and SF 4 in the percentage of TG was 16.7 % and 14.3 % UV-visible

Desempenho do arroz de terras altas com a aplicação de doses de nitrogênio e em sucessão às culturas de cobertura do solo em sistema de plantio direto

A área cultivada no sistema de plantio direto no Brasil tem sido incrementada rapidamente e a cultura do arroz de terras altas pode ser incluída no sistema, em rotação com outras culturas. Outro aspecto importante é a utilização de adubação adequada sendo o nitrogênio um dos nutrientes absorvidos em maior quantidade pelo arroz. Assim, o objetivo do trabalho foi o de avaliar algumas características agronômicas e a produtividade do arroz de terras altas, cv. IAC 202, utilizando-se a combinação de culturas de cobertura - milheto, sorgo granífero, milho, guandu, crotalária, mucuna-preta, além da vegetação espontânea no pousio e doses de N em cobertura - zero, 25, 50, 75, 100 e 125 kg ha-1, no município de Selvíria (MS), nos anos agrícolas 2001/2002 e 2002/2003. Considerando-se os resultados, concluiu-se que a cultura do sorgo é opção viável ao fornecimento de adequada quantidade de massa de matéria seca e ao recobrimento da superfície do solo, mas não para o aumento da produtividade na cultura do arroz em sucessão, em sistema de plantio direto em terras altas; a situação é inversa com a cultura do guandu como planta de cobertura, sendo a produtividade na cultura do arroz em sucessão, em sistema de plantio direto em terras altas, distintamente influenciada pela adubação nitrogenada, em dois anos consecutivos.

Fontes e épocas de aplicação de nitrogênio em trigo em sistema plantio direto no cerrado

O N é um nutriente de suma importância, tendo em vista sua dinâmica no solo e a exigência da cultura, todavia, em muitas situações, o solo é incapaz de suprir todo o requerimento de N das culturas, o que obriga o uso de fertilizantes para a obtenção de produtividade satisfatória. Desse modo, propôs-se este estudo com o objetivo de avaliar diferentes fontes e épocas de aplicação de N em trigo cultivado no sistema plantio direto. O delineamento experimental utilizado foi o de blocos ao acaso disposto em um esquema fatorial 2x6 com quatro repetições. Os tratamentos foram constituídos pela combinação de duas fontes de N: uréia e Entec e seis épocas de aplicação: testemunha (sem N); N na semeadura (S); N 15 dias após a emergência (DAE); N aos 30 DAE; 1/3 do N na S e 2/3 aos 15 DAE; e 1/3 do N na S e 2/3 aos 30 DAE. O experimento foi realizado na área experimental da UNESP - Campus de Ilha Solteira, localizada no município de Selvíria - MS, em solo anteriormente ocupado por vegetação de Cerrado. O N aplicado 30 dias após a emergência propiciou maior produtividade de grãos, entretanto não diferindo estatisticamente da aplicação com 1/3 do N na semeadura + 2/3 do N 30 dias após a emergência.

Doses e épocas de aplicação de nitrogênio na cultura do milho em plantio direto sobre Latossolo Vermelho

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Doses e épocas de aplicação de nitrogênio e teores foliares deste nutriente e de clorofila em feijoeiro

O presente trabalho foi desenvolvido na região de Selvíria (MS) e teve como objetivo avaliar o efeito de diferentes doses e épocas de aplicação de N sobre o teor de clorofila e de N nas folhas do feijoeiro, bem como estabelecer correlações com a produtividade. O delineamento experimental foi de blocos ao acaso, em esquema fatorial 3 x 5, constituído pela combinação de três épocas de aplicação (15, 30 e 15 + 30 dias após a emergência) do fertilizante nitrogenado (uréia) em cobertura e em cinco doses (0; 35; 70; 105 e 140 kg ha-1 de N). Avaliaram-se os teores de clorofila e N das folhas no florescimento pleno e a produtividade. A concentração de clorofila correlacionou-se positivamente com o teor de N nas folhas e com a produtividade de grãos, e o medidor portátil de clorofila mostrou-se promissor para avaliar o estado nutricional do nitrogênio no feijoeiro.

Avaliação de fontes de nitrogênio e épocas de aplicação em cobertura para o cultivo do trigo

The mineral nutrition, mainly to concern to nitrogen, is essential to obtain high productivity in the corn crop. This work was accomplished at experimental station of State University of São Paulo - UNESP - Ilha Solteira Campus, UNESP/FEIS, in Selviria-MS, in a Red dystrophic Latosol (Oxisol), in the agricultural year 2004/05. The objective of this study was to evaluate sources and times of nitrogen application on corn yield. A randomized blocks design was used with four replications, in a 3x5 factorial scheme. The treatments were three sources of nitrogen (Entec - Ammonium sulfonitrate with nitrification inhibitor, Ammonium sulfate and Urea) applied at sowing and/or at covering, stadium of 6-8 leaves completely unfolded, in 5 combinations (0 + 120; 30 + 90; 60 + 60; 90 + 30 and 120 + 0 kg of N ha(-1)). The nitrogen sources as Entec and the combination of 60 kg ha(-1) at sowing and at 6-8 leaf stadium provided the larger N leaf content. The higher grain yield was reached in the treatment that received the higher N doses at covering.

Obtenção de polímeros graftizados de quitosana e estudo das propriedades físico-químicas para aplicação na indústria do petróleo

Chitosan is a biopolymer derived from the shells of crustaceans, biodegradable, inexpensive and renewable with important physical and chemical properties. Moreover, the different modifications possible in its chemical structure generate new properties, making it an attractive polysaccharide owing to its range of potential applications. Polymers have been used in oil production operations. However, growing concern over environmental constraints has prompted oil industry to search for environmentally sustainable materials. As such, this study sought to obtain chitosan derivatives grafted with hydrophilic (poly(ethylene glycol), mPEG) and/or hydrophobic groups (n-dodecyl) via a simple (one-pot) method and evaluate their physicochemical properties as a function of varying pH using rheology, small-angle Xray scattering (SAXS), dynamic light scattering (DLS) and zeta potential. The chitosan derivatives were prepared using reductive alkylation under mild reaction conditions and the chemical structure of the polymers was characterized by nuclear magnetic resonance (1H NMR) and CHN elemental analysis. Considering a constant mPEG/Chitosan molar ratio on modification of chitosan, the solubility of the polymer across a wide pH range (acidic, neutral and basic) could only be improved when some of the amino groups were submitted to reacetylation using the one-pot method. Under these conditions, solubility is maintained even with the simultaneous insertion of n-dodecyl. On the other hand, the solubility of derivatives obtained only through mPEG incorporation using the traditional methodology, or with the ndodecyl group, was similar to that of its precursor. The hydrophilic group promoted decreased viscosity of the polymer solutions at 10 g/L in acid medium. However, at basic pH, both viscosity and thermal stability increased, as well as exhibited a pronounced pseudoplastic behavior, suggesting strong intermolecular associations in the alkaline medium. The SAXS results showed a polyelectrolyte behavior with the decrease in pH for the polymer systems. DLS analyses revealed that although the dilute polymer solutions at 1 g/L and pH 3 exhibited a high density of protonated amino groups along the polymer chain, the high degree of charge contributed significantly to aggregation, promoting increased particle size with the decrease in pH. Furthermore, the hydrophobic group also contributed to increasing the size of aggregates in solution at pH 3, whereas the hydrophilic group helped reduce their size across the entire pH range. Nevertheless, the nature of aggregation was dependent on the pH of the medium. Zeta potential results indicated that its values do not depend solely on the surface charge of the particle, but are also dependent on the net charge of the medium. In this study, water soluble associative polymers exhibit properties that can be of great interest in the petroleum industry

Aplicação de silício em arroz de terras altas irrigado por aspersão

The use of chemical elements considered as beneficial to crops has become common among farmers. The silicon case is interesting, since despite not being essential physiologically for rice crop, it demonstrates that through its absorption it promotes benefits. Therefore, this experiment aimed to evaluate the effect of doses of SiO(2) (0, 150, 300, 450, 600, 750 and 900 kg ha(-1)) at seed sowing time, in two upland rice cultivars (IAC 201 and IAC 202), under sprinkler irrigation, during the agricultural years of 2002/03 and 2003/04 in Selviria, Mato Grosso do Sul State, Brazil. The cultivar IAC 202 can present higher yield than IAC 201, with similar industrial quality and lower laying index. Silicon applications were not sufficient to reduce laying index of IAC 201. In general, silicon application does not interfere in grain productivity and industrial yield of the cultivars used.

Avaliação das propriedades físico-químicas de sistemas a base de carboximetilcelulose e poli (N-isopropilacrilamida) em soluções aquosas para aplicação na indústria do petróleo

Sustainable development is a major challenge in the oil industry and has aroused growing interest in research to obtain materials from renewable sources. Carboxymethylcellulose (CMC) is a polysaccharide derived from cellulose and becomes attractive because it is water-soluble, renewable, biodegradable and inexpensive, as well as may be chemically modified to gain new properties. Among the derivatives of carboxymethylcellulose, systems have been developed to induce stimuli-responsive properties and extend the applicability of multiple-responsive materials. Although these new materials have been the subject of study, understanding of their physicochemical properties, such as viscosity, solubility and particle size as a function of pH and temperature, is still very limited. This study describes systems of physical blends and copolymers based on carboxymethylcellulose and poly (N-isopropylacrylamide) (PNIPAM), with different feed percentage compositions of the reaction (25CMC, 50CMC e 75CMC), in aqueous solution. The chemical structure of the polymers was investigated by infrared and CHN elementary analysis. The physical blends were analyzed by rheology and the copolymers by UV-visible spectroscopy, small-angle X-ray scattering (SAXS), dynamic light scattering (DLS) and zeta potential. CMC and copolymer were assessed as scale inhibitors of calcium carbonate (CaCO3) using dynamic tube blocking tests and chemical compatibility tests, as well as scanning electron microscopy (SEM). Thermothickening behavior was observed for the 50 % CMC_50 % PNIPAM and 25 % CMC_75 % PNIPAM physical blends in aqueous solution at concentrations of 6 and 2 g/L, respectively, depending on polymer concentration and composition. For the copolymers, the increase in temperature and amount of PNIPAM favored polymer-polymer interactions through hydrophobic groups, resulting in increased turbidity of polymer solutions. Particle size decreased with the rise in copolymer PNIPAM content as a function of pH (3-12), at 25 °C. Larger amounts of CMC result in a stronger effect of pH on particle size, indicating pH-responsive behavior. Thus, 25CMC was not affected by the change in pH, exhibiting similar behavior to PNIPAM. In addition, the presence of acidic or basic additives influenced particle size, which was smaller in the presence of the additives than in distilled water. The results of zeta potential also showed greater variation for polymers in distilled water than in the presence of acids and bases. The lower critical solution temperature (LCST) of PNIPAM determined by DLS corroborated the value obtained by UV-visible spectroscopy. SAXS data for PNIPAM and 50CMC indicated phase transition when the temperature increased from 32 to 34 °C. A reduction in or absence of electrostatic properties was observed as a function of increased PNIPAM in copolymer composition. Assessment of samples as scale inhibitors showed that CMC performed better than the copolymers. This was attributed to the higher charge density present in CMC. The SEM micrographs confirmed morphological changes in the CaCO3 crystals, demonstrating the scale inhibiting potential of these polymers

Amostragem do solo em área com cana-de-açúcar após aplicação de corretivos

Este trabalho objetivou avaliar o efeito de dois métodos de amostragem nas propriedades químicas do solo, em área com cana-de-açúcar após tratamentos corretivos de acidez. O primeiro método consistiu na amostragem de solo em 30% dos pontos na posição da linha e 70% na posição da entrelinha (LE). No segundo método, as amostras de solo foram coletadas em 100% dos pontos na posição da entrelinha (E) e da combinação de duas fontes de corretivos, escória e calcário, com níveis de correção do V% para 50, para 75 e para 100, e uma testemunha sem correção. A amostragem do solo pelo método LE superestimou a acidez potencial, enquanto a amostragem do solo na entrelinha apresentou melhor ajuste dos dados para determinação do pH, H + Al, Ca, Mg e V% do solo.