Preparation, characterization and thermal behavior of double selenates of calcium, beryllium and ammonium.

The preparation and thermal decomposition ammonium selenate and calcium and beryllium selenates have been reported previously. However, there are not any information in the literature concerning the thermal decomposition of double selenates of calcium, of beryllium and ammonium. Thermogravimetry (TG), Differential Thermal Analysis (DTA) were used in the studies and characterisation of these compounds.

Study of an organically modified clay: Selective adsorption of heavy metal ions and voltammetric determination of mercury(II)

In this work, a hydrophilic clay, Na-montmorillonite from Wyoming, USA, was rendered organophilic by exchanging the inorganic interlayer cations for hexaclecyltrimethylammonium ions (HDTA), with the formulae of [(CH3)(3)N(C16H33)](+) ion. Based on fact that organo-clay has high affinities for non-ionic organic molecules, 1,3,4-thiadiazole-2,5-dithiol was loaded oil the HDTA-montmorillonite surface, resulting in the 1,3,4-thiadiazole-2,5-dithiol-HDTA-montmorillonite complex (TDD-organo-clay).The following properties of TDD-organo-clay are discussed: selective adsorption of heavy metal ions measured by batch and chromatographic column techniques, and utilization as preconcentration agent in a chemically modified carbon paste electrode (CMCPE) for determination of mercury(II).The main point of this paper is the construction of a selective sensor, a carbon paste electrode modified with TDD-organo-clay, its properties and its application to the determination of mercury(II) ions, as this element belongs to the most toxic metals. The chemical selectivity of this functional group and the selectivity of voltammetry were combined for preconcentration and determination. (c) 2005 Elsevier B.V. All rights reserved.

Infrared spectroscopy investigation of various plasma-deposited polymer films irradiated with 170 keV He+ ions

This work illustrates the advantages of using p-polarized radiation at an incidence angle of 70 degrees in contrast to the conventional unpolarized beam at normal (or near-normal) incidence for the infrared spectroscopic study of polycarbosilane, polysilazane and polysiloxane thin films synthesized by plasma enhanced chemical vapor deposition (PECVD) and subsequently irradiated with 170 keV He+ ions at fluences from 1 x 10(14) to 1 x 10(16) cm(-2). Several bands not seen using the conventional mode could be observed in the polarized mode. (c) 2006 Elsevier B.V. All rights reserved.

New chemical evidence for the ability to generate radical molecular ions of polyenes from ESI and HR-MALDI mass spectrometry

We report here new chemical evidence for the generation of radical molecular ions of compounds with a conjugated pi-system (polyene) in ESI and HR-MALDI mass spectrometry. The oxidation potential of the neutral polyenes was calculated by cyclic-voltammetry and the results compared with those previously published for other complex conjugated compounds that have also been shown to form M.+ in ESI-MS. This study clearly demonstrates the correlation between the oxidation potential and the formation of the M.+ for the polyenes studied.

Leaching of nitrate and ammonium from cover crop straws as affected by rainfall

Nitrogen (N) mineralization dynamics in no-till systems is affected, among other factors, by N amount and quality in the mulch and by climatic conditions. Leaching of NO3-N and NH4-N from six plant species used as soil cover crops in tropical environments were evaluated when the straw was submitted to rainfall after chemical desiccation. Millet (Pennisetum glaucum), guinea sorghum (Sorghum vulgare), black oat (Avena strigosa), triticale (Triticum secale), Indian hemp (Crotalaria juncea), and brachiaria (Brachiaria decumbens) were grown in a greenhouse, in Botucatu-SP, Brazil. Forty-five days after emergence, the plants were cut at the root collar, oven-dried, and submitted to simulated rainfalls of 4.4, 8.7, 17.04, 34.9, and 69.8 mm, considering an amount of straw equivalent to 8 t ha(-1) of dry matter. The amounts of N-NO3- extracted from the straw by rainwater were very small. However, accumulated rainfall around 70 mm caused ammonium leaching ranging from 2.5 to 9.5kg ha(-1), depending on the species. Plant residues of triticale and black oat (grasses) and Indian hemp (legume) showed high N leaching intensity with the first rains after chemical desiccation. The amount of N leached from straw was highly correlated with N tissue content.

Structure of luminescent mono and di-urethanesil nanocomposites doped with Eu3+ ions

A structure modeling of two families of sol-gel derived Eu3+-doped organic/inorganic hybrids based on the results of small-angle X-ray scattering experiments is reported. The materials are composed of poly(oxyethylene) chains grafted at one or both ends to siloxane groups and are called mono- and di-urethanesils, respectively. A theoretical function corresponding to a two-level hierarchical structure model fits well the experimental Scattering curves. The first level corresponds to small siloxane clusters embedded in a polymeric matrix. The secondary level is associated to the existence of siloxane cluster rich domains surrounded by a cluster-depleted polymeric matrix. Results show that increasing europium doping favors the growth of the secondary domains. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Structural study of a series of synthetic goethites obtained in aqueous solutions containing cadmium(II) ions

The capacity of goethite for Cd-II substitution has been explored in a series of synthetic samples prepared from Fe-III and Cd-II nitrate solutions aged 21 days in alkaline media. The total metal content ([ Fe] + [ Cd]) was 0.071 M in all preparations. The samples have been characterized by chemical and X-ray diffraction analysis; the morphology of the solids is described. The cell parameters for all samples were obtained by the Rietveld fits to the X-ray diffraction data. Refined structures show that for samples prepared at the final molar ratio mu(Cd)less than or equal to5.50 (expressed as mu(Cd) = 100X[Cd]/[Cd] + [Fe]), a (Cd, Fe)-goethite is the only crystalline product. In these samples, the unit cell parameters increased as a function of Cd concentration, indicating Cd incorporation in the structural frame. At the preparative ratio, mu(Cd)=7.03, the incorporation of Cd in the goethite structure is drastically reduced and a probable Cd-substituted hematite is formed together with the Fe,Cd-goethite. (C) 2003 International Centre for Diffraction Data.

Indirect determination of chloride and sulfate ions in alcohol fuel by capillary electrophoresis

A capillary zone electrophoresis method using indirect UV detection for the analysis of chloride and sulfate in alcohol fuel samples was developed. The anions were analyzed in less than 3 min using an electrolyte containing 10 mmol 1(-1) chromate and 0.75 mmol 1(-1) hexamethonium bromide (HMB) as electroosmotic flow modifier. Coefficients of variation were better than 0.6% for migration time (n = 10) and between 2.05 and 2.82% for peak area repeatabilities. Analytical curves of peak area versus concentration in the range of 0.065-0.65 mg kg(-1) for chloride and 0.25-4.0 mg kg(-1) for sulfate were linear with coefficients of correlation higher than 0.9996. The limits of detection for sulfate and chloride were 0.033 and 0.041 mg kg(-1), respectively. Recovery values ranged from 85 to 103%. The method was successfully applied for the quantification of sulfate and chloride in five alcohol fuel samples. The concentration of sulfate varied from 0.45 to 3.12 mg kg(-1). Chloride concentrations were below the method's LOD.

Sorption and preconcentration of metal ions in ethanol solution with a silica gel surface chemically modified with benzimidazole

The adsorption isotherms of MCl(2) (M = Mn, Ni, Cu, Zn and Cd) and FeCl3 by silica gel chemically modified with benzimidazole molecules (= SI(CH2)(3)-NC7H5N) were studied in ethanol solution at 298 K. A column made of modified silica was used to adsorb and preconcentrate the above metal ions from ethanol solution. Elution was done with 0.1 M hydrochloric acid in an ethanol/water mixture having a mole fraction of water of 0.8. The material was applied in the preconcentration of metal ions from commercial ethanol normally used as engine fuel.

ISOLATION OF BABESIA-BIGEMINA AND BABESIA-BOVIS MEROZOITES BY AMMONIUM-CHLORIDE LYSIS OF INFECTED ERYTHROCYTES

1. We describe the isolation of viable merozoites from erythrocytes infected with Babesia bovis or Babesia bigemina organisms by ammonium chloride lysis.2. Parasite morphology was examined by both light and transmission electron microscopy. Erythrocyte-free parasites maintain their viability and infectivity, retain their antigenicity and are suitable for use in the indirect fluorescent antibody assay.

Sorption and preconcentration of metal ions on silica gel modified with 2,5-dimercapto-1,3,4-thiadiazole

Silica gel, chemically modified with 2,5-dimercapto-1,3,4-thiadiazole [=Si(CH2)(3)-NC2HNS3], abbreviated as SiB, was used to adsorb metal ions from ethanol by both batch and column techniques. Elution of Cu(II) was done with a solvent mixture of acetone and hydrochloric acid (9:1 v/v). Zn(II), Cd(II), Ni(II), Pb(II), Co(II) and Fe(III) were eluted with 0.5 mol l(-1) HC1 in ethanol solution. The modified silica was applied in the preconcentration of metal ions from commercial ethanol, normally used as engine fuel. The method is suitable for quantifying these metals at low mu g l(-1) levels.

4f-4f intensities of the Tm3+ ions in fluoroindate glasses: the influence of third-order effects through odd intensity parameters

In this work an analysis of the phenomenological Omega(lambda) intensity parameters for the Tm3+ ion in fluoroindate glass is made using the standard Judd-Ofelt theory, and a modified oscillator strength taking into account odd-order contributions is utilized. Different sets of phenomenological intensity parameters Omega(lambda) (lambda=1,2,3,4,5,6) are discussed. The set of better quality is used to analyze the influence of third-order effects through odd intensity parameters in the new approximation. Fluoroindate glasses of compositions (40-x)InF3-20ZnF(2)-20SrF(2)-16BaF(2)-2GdF(3)-2NaF-xTmF(3) with x=1, 2 and 3 mol% were prepared, and the absorption spectra at room temperature in the spectral range from 300 to 2500 nm were obtained. The experimental oscillator strengths determined from the area under the absorption band are compared to the calculated ones. (C) 1998 Elsevier B.V. S.A.

Synthesis, characterisation and thermal behaviour of solid state compounds of 4-methylbenzylidenepyruvate with some bivalent metal ions

Solid state M-4-Me-BP compounds, where M stands for bivalent Mn, Fe, Co, Ni, Cu, Zn, Pb and 4-Me-BP is 4-methylbenzylidenepyruvate, have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, elemental analysis, and complexometry were used to characterise and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, thermal stability and thermal decomposition of the isolated complexes. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Effects of the magnesium and chloride ions and shikimate on the structure of shikimate kinase from Mycobacterium tuberculosis

Bacteria, fungi and plants can convert carbohydrate and phosphoenolpyruvate into chorismate, which is the precursor of various aromatic compounds. The seven enzymes of the shikimate pathway are responsible for this conversion. Shikimate kinase (SK) is the fifth enzyme in this pathway and converts shikimate to shikimate-3-phosphate. In this work, the conformational changes that occur on binding of shikimate, magnesium and chloride ions to SK from Mycobacterium tuberculosis (MtSK) are described. It was observed that both ions and shikimate influence the conformation of residues of the active site of MtSK. Magnesium influences the conformation of the shikimate hydroxyl groups and the position of the side chains of some of the residues of the active site. Chloride seems to influence the affinity of ADP and its position in the active site and the opening length of the LID domain. Shikimate binding causes a closing of the LID domain and also seems to influence the crystallographic packing of SK. The results shown here could be useful for understanding the catalytic mechanism of SK and the role of ions in the activity of this protein.

Influence of sugar cane burning on aerosol soluble ion composition in Southeastern Brazil

Seasonal variability in the major soluble ion composition of atmospheric particulate matter in the principal sugar cane growing region of central São Paulo State indicates that pre-harvest burning of sugar cane plants is an important influence on the regional scale aerosol chemistry. Samples of particulate matter were collected between April 1999 and February 2001 in coarse (> 3.5 mum) and fine (< 3.5 mum) fractions, and analysed for HCOO-, CH3COO-, C2C42-, SO42- . Results indicated that the principal sources of the aerosols investigated NO3-, Cl-, Na+, K+, NH4+, Mg2+ and Ca2+ were local or regional in nature (scale of tens to a few hundreds of km), and that differences between air masses of varying origins were small. Fine particles were typically acidic, containing secondary nitrates, sulphates and organic species. Coarse fraction concentrations were mainly influenced by physical parameters (wind speed, movement of vehicles and surface condition) affecting rates of re-suspension, although secondary nitrate and sulphate were also present in the larger particles.Concentrations of all measured species except sodium and chloride were higher during the burning season. Although concentrations were lower than often found in polluted urban environments, the massive increases during much of the year, due to a single anthropogenic activity (sugar cane burning) are indicative of a very large perturbation of the lower troposphere in the region relative to the natural condition. These aerosols are suspected of promoting respiratory disease. They also represent an important mechanism for the tropospheric transport of species relevant to surface acidification (sulphates, nitrates, ammonium and organic acids) and soil nutrient status (potassium, nitrogen, ammonium, calcium), so their impact on fragile natural ecosystems (following deposition) needs to be considered. (C) 2004 Elsevier Ltd. All rights reserved.