New chelate complexes of trivalent Y and lanthanides (Eu, Ho, Yb) with a triazene N-oxide: Synthesis, structural characterization and luminescence properties

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Research of new mixed-chelate copper complexes with quinoxaline N 1,N 4,-dioxide derivatives and alanine as ligands, potential antimycobacterial agents

Three new mixed-chelate copper complexes with 3-aminoquinoxaline-2-carbonitrile N 1,N 4-dioxide derivatives and alanine as ligands were synthesized in solid state. The spectroscopic characterization (FTIR, EPR, UV-Vis) showed that copper coordinated through the amine and the N-oxide groups of the quinoxaline derivatives and the amine and carboxylate moieties from alanine forming a dimeric species. The tree complexes showed in vitro activity against M. tuberculosis H 37Rv (ATCC 27294) similar to that of ethambutol while they are inactive against E. coli and S. aureus.

A new palladium chelate compound for determination of sulfide

A new palladium chelate compound is described for the determination of sulfide in aqueous samples. The reagent, bis(2-aminobenzoate)palladium(II) (PdA 2), was prepared by reaction of tetrachloropalladate (PdCl 4 -) with 2-aminobenzoic acid. The compound was characterized by infrared spectroscopy and CHN elemental analysis. The measurement was based on the selective reaction of PdA 2 with sulfide in an aqueous medium, which quantitatively produced fluorescent 2-aminobenzoate (λ ex=245nm, λ em=410nm). The analytical response was linear in the range 0.10-20.0μmol (S 2-) L -1 (r>0.99), with a limit of detection of 0.075μmolL -1 and repeatability (RSD) of 3.4%. There was no interference from CO 3 2-, NO 3 -, Cl -, SO 4 2-, Br -, NO 2 -, K +, NH 4 +, Na +, citrate or S 2O 8 2-. The fluorescence intensity decreased in the presence of H 3CCOO -, PO 4 3- and SCN -, while OH - caused a positive interference. The new fluorescent compound was successfully applied for the determination of sulfide in synthetic wastewater and natural water sample. The advantages of the proposed palladium chelate are absence of toxic by-products, simple synthesis procedure of reagent and yield reaction of about 85%, easy handling and fast acquirement of analytical signal. © 2012 Elsevier B.V.

Manganês e potencial fisiológico de sementes de soja

O trabalho teve por objetivo avaliar a influência de diferentes fontes e modos de aplicação de manganês, em plantas de soja, sobre o potencial fisiológico das sementes produzidas e a massa de mil sementes. Os tratamentos constaram de fontes de manganês aplicadas via solo (MnSO4.4H2O e Oxi-sulfato Mn) e via foliar (MnSO4.4H2O, Quelado Cl-, Quelado NO3- e Quelado SO4(2-)); para as sementes produzidas, determinaram-se a massa de mil sementes, a germinação e o vigor (envelhecimento acelerado e condutividade elétrica). Diante dos resultados obtidos, concluiu-se que a aplicação de manganês exerceu influência positiva sobre a massa das sementes de soja produzidas e que o estado nutricional das plantas, em relação ao manganês, não influenciou o potencial fisiológico das sementes produzidas.

Organic and inorganic sources of zinc, copper and selenium in diets for dairy cows: intake, blood metabolic profile, milk yield and composition

The present study was carried out with the objective of evaluating the effects of feeding dairy cows with organic or inorganic sources of zinc (Zn), copper (Cu) and selenium (Se) on blood concentrations of these minerals, blood metabolic profiles, nutrient intake and milk yield and composition. Nineteen Holstein cows were selected and randomly assigned to two groups for receiving organic (n = 9) or inorganic (n = 10) sources of Zn, Cu and Se from 60 days before the expected date of calving to 80 days of lactation. Samples of feed, orts and milk were collected for analysis. Body condition score (BCS) was determined and blood samples were collected for analysis of Zn, Cu and Se concentrations, as well as for metabolic profile. Supplying organic or inorganic sources of Zn, Cu, and Se did not affect dry matter and nutrient intake, blood metabolic profile, milk yield and composition, plasma concentration of these minerals, and BCS or change the BCS in cows from 60 days before the expected date of calving to 80 days of lactation. An effect of time was observed on all feed intake variables, plasma concentrations of Zn and Se, milk yield, milk protein content, BCS and change in BCS.

Phytase immobilization on modified electrodes for amperometric biosensing

Phytase (myo-inositol hexaphosphate phosphohydrolase) and phytic acid (myo-inositol hexaphosphate) play an important environmental role, in addition to being a health issue in food industry. Phytic acid is antinutritional due to its ability to chelate metal ions and may also react with proteins decreasing their bioavailability. In this work, we produced biosensors with phytase immobilized in Layer-by-Layer (LbL) films, which could detect phytic acid with a detection limit of 0.19 mmol L-1, which is sufficient to detect phytic acid in seeds of grains and vegetables. The biosensosrs consisted of LbL films containing up to eight bilayers of phytase alternated with poly(allylamine) hydrochloride (PAH) deposited onto an indium-tin oxide (ITO) substrate modified with Prussian Blue. Amperometric detection was conducted in an acetate buffer solution (at pH 5.5) at room temperature, with the biosensor response attributed to the formation of phosphate ions. In subsidiary experiments with the currents measured at 0.0 V (vs. SCE), we demonstrated the absence of effects from some interferents, pointing to a good selectivity of the biosensor. (c) 2007 Elsevier B.V. All rights reserved.

Development on polymeric precursor routes to produce superconducting nanoparticles

The well-known polymeric precursor route is a simple and low-cost sol-gel method based on the preparation of an aqueous precursor solution of metals followed by the addition of a water-soluble polymer. This method consists of a polyesterification process between a metal chelate complex by using a hydroxycarboxylic acid and a polyhydroxy alcohol. In this work, citric acid (CA), tartaric acid (TA) and ethylenediaminetetraacetic acid (EDTA) are used as the hydroxycarboxylic acid and ethylene glycol (EG) is used as the polyhydroxy alcohol. The effects of the precursor pH solution, time and temperature of polymerization step as well as the combination of different chelating agents in order to obtain nanoscopic YBa2Cu3Oy samples were traced. (c) 2007 Elsevier B.V. All rights reserved.

Foliar Fertilization on pineapple quality and yield

Poucos são os estudos desenvolvidos com a aplicação via foliar de micronutrientes, na cultura do abacaxi. Este trabalho teve como objetivo avaliar os efeitos de B e Zn, em forma de quelato, ácido ou sal, via foliar, buscando-se obter respostas sobre os efeitos na produtividade e qualidade dos frutos. O experimento foi realizado em Guaraçaí (SP), em solo com textura média. Foram utilizadas mudas tipo filhote, da cultivar Smooth Cayenne (Havaiano). O delineamento experimental adotado foi o de blocos ao acaso, com quatro repetições, utilizando-se fontes para fornecer, em cada aplicação, 110 g ha-1de B e 250 g ha-1de Zn. Foram realizadas duas pulverizações foliares, aos 7 e 9 meses após o plantio. As fontes de B e Zn não exerceram efeito nos teores de sólidos solúveis totais, acidez titulável, diâmetro médio do fruto, comprimento do fruto sem coroa e índice de maturação. Apenas os teores de B, Zn e K, na folha, foram influenciados pelos tratamentos utilizados.

Biodisponibilidade de ferro em diferentes compostos para leitões desmamados aos 21 dias de idade

Avaliou-se a biodisponibilidade de ferro de diferentes compostos visando sua utilização em dietas para leitões desmamados. Utilizaram-se 44 leitões (7 não-anêmicos e 37 anêmicos) desmamados aos 21 dias de idade (7,3 ± 1,8 kg) e distribuídos em dois grupos: grupo não-anêmico e grupo anêmico. Durante sete dias, os animais do grupo não-anêmico receberam dieta com FeSO4.7H2O (sulfato ferroso hepta-hidratado) na dose de 100 mg/kg e os do grupo anêmico, dieta sem ferro (<15 mg/kg ração). No sétimo dia, depois de determinada a concentração de hemoglobina sanguínea e diagnosticada a anemia, os leitões foram agrupados segundo o produto do peso (kg) × hemoglobina (g/dL) e alojados individualmente, durante 13 dias, em gaiolas para estudos de digestibilidade, onde foram alimentados com seis rações à base de milho e leite em pó: três rações-padrão com FeSO4.7H2O em quantidade equivalente a 80, 150 e 200 mg Fe/kg de ração; duas rações experimentais com ferro (150 mg/kg) na forma de FeSO4 microencapsulado com carboximetilcelulose ou de ferro quelado com metionina; e uma controle com ferro (100 mg/kg). O consumo de ração foi medido diariamente. Nos dias 0, 3, 6, 9 e 13 do período de repleção, os animais foram pesados para avaliação do desempenho e o sangue foi coletado para determinação da concentração de hemoglobina. Ao final do ensaio, os animais foram sacrificados e o fígado foi coletado para determinação das concentrações de ferro total, ferro heme e ferro não-heme. As concentrações hepáticas de ferro heme, ferro não-heme e ferro total não diferiram entre os animais, entretanto, os do grupo controle apresentaram excesso de ferro total no fígado, relacionado à dose de ferro injetada nos leitões após o desmame. em comparação ao FeSO4.7H2O não encapsulado, os compostos de ferro microencapsulado com carboximetilcelulose e de ferro quelado com metionina promovem melhor conversão alimentar em leitões desmamados.

Micromorphology and spectroscopic characteristics of organic matter in waterlogged podzols of the upper Amazon basin

In waterlogged environments of the upper Amazon basin, organic matter is a major driver in the podzolisation of clay-depleted laterites, especially through its ability to weather clay minerals and chelate metals. Its structure in eight organic-rich samples collected at the margin and in the centre of the podzolic area of a soil sequence was investigated. The samples illustrate the main steps in the development of waterlogged podzols and belong either to eluviated topsoil A horizons or to illuviated subsoil Bhs, Bh and 2BCs horizons. Organic matter micromorphology was described, and the overall molecular structure of their clay size fractions was assessed using Fourier transform infrared (FTIR) spectroscopy and cross polarization/magic angle spinning (CP/MAS) C-13 nuclear magnetic resonance (NMR). Organic features of the horizons strongly vary both vertically and laterally in the sequence. Topsoil A horizons are dominated by organic residues juxtaposed to clean sands with a major aliphatic contribution. In the subsoil, numerous coatings, characteristic of illuviation processes, are observed in the following horizons: (i) At the margin and bottom parts of the podzolic area, dark brown organic compounds of low aromacity with abundant oxygen-containing groups accumulate in Bhs and 2BCs horizons. Their spectroscopic features agree with the observation of cracked coatings in 2BCs and the presence of organometallic complexes, whose abundance decreases towards low lying positions. (ii) By contrast, black organic compounds of high aromacity with few chelating functions accumulate as coatings and infills in the overlying sandy Bh horizon of well-expressed waterlogged podzols. (c) 2008 Elsevier B.V. All rights reserved.

Synthesis and characterization of antimony tartrate for ceramic precursors

Synthesis and characterization of antimony tartrate used as a precursor of ceramic powders obtained by Pechini's method were carried out. Antimony tartrate was chosen as a substitute for the antimony citrate commonly used in this chemical processing, because of difficulties in preparing the citrate. FTIR and TGA/DTA analysis showed that antimony tartrate, H-2[Sb-2(C4H2O6)(2)]. forms a polymeric structure. The procedure described indicates that the antimony chelate obtained is adequate for Pechini's method.

Preparação e caracterização do complexo sólido de estanho(II)-EDTA e influência do tratamento térmico sobre a morfologia do resíduo SnO2

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Produtividade e desenvolvimento da cana-planta e soca em função de doses e fontes de manganês

A cana-de-açúcar possui grande importância econômico-social e política para o Brasil. Este trabalho teve como objetivo avaliar o efeito de doses e fontes de manganês nessa cultura. O experimento foi realizado no sítio Fujimoto, área administrada pela Destilaria Vale do Paraná S/A Álcool e Açúcar, no município de Suzanápolis, SP. O delineamento experimental utilizado foi o de blocos ao acaso no esquema fatorial 5 x 3, sendo cinco doses de Mn (0; 2,5; 5,0; 7,5; e 10,0 kg ha-1) e três fontes (quelato, FTE e sulfato de manganês), aplicadas no sulco de plantio, em quatro repetições. As parcelas foram constituídas por quatro linhas de 5 m de comprimento e espaçadas 1,5 m. A variedade de cana-de-açúcar utilizada foi a RB 86-7515, realizando-se dois cortes. As fontes de Mn proporcionaram semelhantes produtividades de colmos, tanto da cana-planta quanto da primeira cana-soca. O quelato de Mn proporcionou maior número de colmo por metro de sulco na cana-soca. As doses de Mn não influenciaram a produtividade de colmos da cana-planta e da cana- soca, porém aumentaram o número de internódios e o diâmetro de colmo na cana-planta até as doses de 6,9 e 6,6 kg ha-1 de Mn, respectivamente.

Adubação foliar. I. Épocas de aplicação de fósforo na cultura da soja

The search for new alternatives in order to increase soybeans productivity has been constant objective of researchers and farmers. The crop responses to phosphorus application in the soil are well defined, being this nutrient very important on its development and yield. The leaf fertilization on this crop appears as a new rationale option, mainly when the plant nutrient levels are low. So, this work aimed to study the effect of phosphorus leaf fertilization, applied at different plant stage, including: V5, R1, R4, V5 + R1, V5 + R4, R1 + R4, V5 + R1 + R4, V5 + R1 + R4 + R6 and test plot. The experiment was installed in a soybeans crop, Monarca cultivar, at Palmital Farm, Ijaci county, Minas Gerais state, Brazil, using a totally randomized design, with 9 treatments and 3 replications. The chelate Quimifol P30 in liquid form with 30% of the nutrient soluble in CNA + water in the, with doses of 21. ha(-1), was utilized as phosphorus source, using the applications performed with a constant pressure CO(2)-nebulizer. The different epochs of phosphorous application significantly altered the grains yield, proportioning significant increases, up to 16% for the V5, V5 + R1, V5 + R4, V5 + R1 + R4, V5 + R1 + R4 + R6 epochs, when compared to the test plot, clearly expressing the positive effect of these applications at V5 stage. The plant height, first legume insertion, and lodging index characteristics were not significantly altered by the different epochs evaluated. It was observed significant response for the nutrient leaf amounts only in the case of K and Zn indices, exclusively in the V5 + R4, and in the V5, V5 + R1 and V5 + R1 + R4 + R6 treatments, respectively.

Tin(II)-EDTA complex: kinetic of thermal decomposition by non-isothermal procedures

Tin on the oxide form, alone or doped with others metals, has been extensively used as gas sensor, thus, this work reports on the preparation and kinetic parameters regarding the thermal decomposition of Sn(II)-ethylenediaminetetraacetate as precursor to SnO2. Thus, the acquaintance with the kinetic model regarding the thermal decomposition of the tin complex may leave the door open to foresee, whether it is possible to get thin film of SnO2 using Sn(II)-EDTA as precursor besides the influence of dopants added.The Sn(II)-EDTA soluble complex was prepared in aqueous medium by adding of tin(II) chloride acid solution to equimolar amount of ammonium salt from EDTA under N-2 atmosphere and temperature of 50degreesC arising the pH similar to 4. The compound was crystallized in ethanol at low-temperature and filtered to eliminate the chloride ions, obtaining the heptacoordinated chelate with the composition H2SnH2O(CH2N(CH2COO)(2))(2).0.5H(2)O.Results from TG, DTG and DSC curves under inert and oxidizing atmospheres indicate the presence of water coordinated to the metal and that the ethylenediamine fraction is thermally more stable than carboxylate groups. The final residue from thermal decomposition was the SnO2 characterized by X-ray as a tetragonal rutile phase.Applying the isoconversional Wall-Flynn-Ozawa method on the DSC curves, average activation energy: E-a = 183.7 +/- 12.7 and 218.9 +/- 2.1 kJ mol(-1), and pre-exponential factor: log A = 18.85 +/- 0.27 and 19.10 +/- 0.27 min(-1), at 95% confidence level, could be obtained, regarding the loss of coordinated water and thermal decomposition of the carboxylate groups, respectively. The E-a and logA also could be obtained applying isoconventional Wall-Flynn method on the TG curves.From E-a and log A values, Dollimore and Malek procedures could be applied suggesting R3 (contracting volume) and SB (two-parameter model) as the kinetic model to the loss of coordinated water (177-244degreesC) and thermal decomposition of the carboxylate groups (283-315degreesC), respectively. Simulated and experimental normalized DTG and DSC curves besides analysis of residuals check these kinetic models. (C) 2003 Elsevier B.V. All rights reserved.