A thermal analysis study of dithizone and dithizonates of mercury, silver and bismuth

Foram preparados os ditizonatos de Hg (I), Ag (I) e Bi (III). Termogravimetria (TG), termogravimetria derivada (DTG), calorimetria exploratória diferencial (DSC), difratometria de raios X pelo método do pó e análise elementar foram usados para caracterizar e para estudar a estabilidade térmica e a decomposição térmica da ditizona e destes ditizonatos.

SILVER DISSOLUTION ON COPPER-BASED ALLOYS

Electrical resistivity measurements and scanning electron microscopy was used to study the dissolution of silver on Cu-Ag and Cu-Al-Ag alloys. The results seem to indicate that the dissolution temperature is affected by the addition of aluminium.

Silver as internal standard for simultaneous determination of Cd and Pb in whole blood by electrothermal atomic absorption spectrometry

The use of internal standardization for simultaneous atomic absorption spectrometry (SIMAAS) was investigated for Cd and Pb determination in whole blood. The comparison of thermochemical and physicochemical parameters allowed the selection of Ag, Bi, and Tl as internal standard candidates. Correlation graphs, plotted from the normalized absorbance signals (n = 20) of internal standard (axis y) versus analyte ( axis x), precision and accuracy were used to select Ag as the most appropriate internal standard. Blood samples were diluted (1 + 9) with 0.11% (m/v) Triton X-100 + 1.1% (v/v) HNO3 + 0.28% (m/v) NH4H2PO4 + 10 mug L-1 Ag+. Pyrolysis and atomization temperatures for the optimized heating program were 550 and 1700 degreesC, respectively. Characteristic masses based on integrated absorbance were 1.68 +/- 0.01 pg for Cd and 30.3 +/- 0.1 pg for Pb. The detection limits (DL) were 0.095 +/- 0.001 mug L-1 and 0.86 +/- 0.01 mug L-1 for Cd and Pb, respectively. The mean RSD for all determinations was the same for Cd (13 +/- 9%) with or without Ag as internal standard ( IS). on the other hand, the use of Ag as IS improved the RSD for Pb from 3.6 +/- 4.0% to 2.2 +/- 2.0%. An effective contribution of the internal standard Ag was verified in the recoveries of spiked samples (0.5 mug L-1 Cd2+ and 5.0 mug L-1 Pb2+). The mean recoveries were 81 +/- 8% and 91 +/- 4% for Cd, and 80 +/- 11% and 93 +/- 6% for Pb without and with IS correction, respectively. This is the first application of IS for a simultaneous determination by SIMAAS.

Evolutionary chromosomal differentiation among four species of Conoderus Eschscholtz, 1829 (Coleoptera, Elateridae, Agrypninae, Conoderini) detected by standard staining, C-banding, silver nitrate impregnation, and CMA(3)/DA/DAPI staining

The speciose Brazilian Elateridae fauna is characterized by high karyotypic diversity, including one species (Chalcolepidius zonatus Eschscholtz, 1829) with the lowest diploid number within any Coleoptera order. Cytogenetic analysis of Conoderus dimidiatus Germar, 1839, C. scalaris (Germar, 1824,) C. ternarius Germar, 1839, and C. stigmosus Germar, 1839 by standard and differential staining was performed with the aim of establishing mechanisms of karyotypic differentiation in these species. Conoderus dimidiatus, C. scalaris, and C. ternarius have diploid numbers of 2n(male) = 17 and 2n(female) = 18, and a X0/XX sex determination system, similar to that encountered in the majority of Conoderini species. The karyotype of C. stigmosus was characterized by a diploid number of 2n=16 and a neoXY/neoXX sex determination system that was highly differentiated from other species of the genus. Some features of the mitotic and meiotic chromosomes suggest an autosome/ancestral X chromosome fusion as the cause of the neoXY system origin in C. stigmosus. C-banding and silver impregnation techniques showed that the four Conoderus species possess similar chromosomal characteristics to those registered in most Polyphaga species, including pericentromeric C band and autosomal NORs. Triple staining techniques including CMA(3)/DA/DAPI also provided useful information for differentiating these Conoderus species. These techniques revealed unique GC-rich heterochromatin associated with NORs in C. scalaris and C. stigmosus and CMA(3)-heteromorphism in C. scalaris and C. ternarius.

Pattern of nucleolar activity during spermiogenesis in triatomines (Heteroptera, Reduviidae) as analysed by silver staining

Nucleoli are the sites of biosynthesis of ribosomal precursors. In this work the nucleolar activity at interphase and the meiotic cells of the testis in five species of triatomines were analysed by means of silver staining. Several nucleolar blocks in the polyploid nuclei of testicular tubules were observed, whereas only one nucleolar body could be seen in the spermatogonial nuclei of all five species. A single nucleolar body was evident in the 'confused stage' of Triatoma brasiliensis, T. delpontei, T. lecticularia and T. rubrovaria, while T. sordida presented two nucleolar dots. The existence of small, silver-stained dots in some metaphase I chromosomes of T. brasiliensis and T. sordida is reported. The number of nucleolar dots present in spermatids of each species varied within and among species. It is suggested that in addition to providing information on rRNA biosynthesis, studies of nucleolar organizing activity can also be important sources of data on differentiation patterns and species development.

Processing and properties of Ag/BSCCO PIT tapes containing different proportions of silver metal powder

Monofilamentary tapes (150 pm thickness) were prepared by swaging and rolling silver tubes containing the Bi:2212 ceramic (granulation below 20 mum) and the silver powder (about 0.8 mum). The study has been made, among other samples, on tapes with nominal proportions of 0, 10 and 20 wt.% of silver. The samples were characterized by SEM, and by electrical measurements under varying applied magnetic field. The measurements of J(c) showed that the addition of 10 wt.% silver powder is very beneficent to this property, doubling the obtained values at 60 K, while the 20 wt.% tape presented very low J(c). The tape with no silver content showed to have a J(c) as high as 2.2 x 10(5) A/cm(2), at 4.2 K, zero applied magnetic field. (C) 2004 Elsevier B.V. All rights reserved.

Mass fractal characteristics of sonogels prepared from sonohydrolysis of tetraethoxysilane with additions of dimethylformamide

Wet silica gels with similar to 1.4 x 10(-3) mol SiO2/cm(3) and similar to 90 vol.% liquid phase were prepared from the sonohydrolysis of tetraethoxysilane (TEOS) with different additions of dimethylformamide (DMF). Aerogels were obtained by CO2 supercritical extraction. The samples were studied mainly by small-angle X-ray scattering (SAXS) and nitrogen adsorption. Wet gels exhibit a mass fractal structure with fractal dimension D increasing from 2.23 to 2.35 and characteristic length xi decreasing from similar to 9.4 nm to similar to 5.1 nm, as the DMF/TEOS molar ratio is increased from 0 to 4. The supercritical process apparently eliminates some porosity, shortening the fractality domain in the mesopore region and developing an apparent surface/mass fractal (with correlated mass fractal dimension D-m similar to 2.6 and surface fractal dimension D-s similar to 2.3) in the micropore region. The fundamental role of the DMF addition on the structure of the aerogels is to diminish the porosity and the pore mean size, without, however, modify substantially the specific surface area and the average size of the silica particle of the solid network. (c) 2006 Elsevier B.V. All rights reserved.

A kinetic model for the ultrasound catalyzed hydrolysis of solventless TEOS-water mixtures and the role of the initial additions of ethanol

The acid and ultrasound catalyzed hydrolysis of solventless TEOS-water mixtures are studied, as a function of the initial additions of ethanol to the mixtures, by means of flux calorimetry measurements. A device was specially designed for this purpose. Under acid conditions, our proposed method has been able to resolve hydrolysis from other condensation reactions, by detecting the exothermal hydrolysis reaction heat. The process has been explained by a dissolution and reaction mechanism. Ultrasound forces the dissolution process to start the reaction. The alcohol produced in the reaction helps the dissolution process to further enhance the hydrolysis. Initial amounts of pure ethanol added to the mixtures shorten the start time of the reaction, due to an additional effect of dissolution, and diminish the reaction rate, as a result of the solvent dilution effect. Our dissolution and reaction mechanism modeling describes the main points arising from the experimental data and yields k(H) = 0.24 M(-1) min(-1) for the second-order hydrolysis rate constant at 39 degrees C.

Complete staining of nerve fiber and myoneural junctions with acetylthiocholine and silver

We describe a combined stain for simultaneous demonstration of the preterminal axons and cholinesterase activity at myoneural junctions of mammalian muscles. This technique employs acetylthiocholine iodide as the substrate for cholinesterase activity and silver nitrate impregnation of preterminal axons. The procedure is rapid, simple and uses fresh muscles. Intramuscular nerves, preterminal axons and myoneural junctions are stained simultaneously brown or black with minimal background staining of connective tissue and muscle fibers.

Potentiometric determination of saccharin in commercial artificial sweeteners using a silver electrode

A simple, precise, rapid and low-cost potentiometric method for saccharin determination in commercial artificial sweeteners is proposed. Saccharin present in several samples of artificial sweeteners is potentiometrically titrated with silver nitrate solution using a silver wire as the indicator electrode, coupled to a titroprocessor. The best pH range was from 3.0 to 3.5 and the detection limit of sodium saccharin was 2.5 mg/ml. Substances normally found along with saccharin in several commercial artificial sweeteners such as maltodextrin, glucose, sucrose, fructose, aspartame, cyclamate, caffeine, sorbitol, lactose, nitrate, methyl- and n-propyl-p-hydroxybenzoate, benzoic, citric and ascorbic acids do not interfere even in significant amounts (e.g. 20 excess relative to saccharin). Chloride ion interferes when present in concentrations larger than 10 mg l(-1); this interference is eliminated with previous extraction of the sweetener from the aqueous medium with ethyl acetate. The results obtained by applying the proposed method compared very favorably with those given by the HPLC method recommended by the FDA. (C) 2003 Elsevier Ltd. All rights reserved.

X-ray powder diffraction analysis of a silver(I)-aspartame complex

Synchrotron X-ray powder diffraction (XRPD) data were collected for the silver(I)-aspartame complex [Ag(C14H17N2O5)]center dot 1/2 H2O. The complex was obtained from a stoichiometric mixture of aspartame (3-amino-N-(alpha-carboxyphenethyl)-succinamic acid N-methyl ester, C14H18N2O5), Na2CO3, and AgNO3. Indexing using Crysfire and Chekcell proposed an orthorhombic unit cell with space group P222(1). The lattice parameters are a = 12.4750(1) angstrom, b = 21.60614(14) angstrom, and c = 4.88888(9) angstrom. (C) 2006 International Centre for Diffraction Data.

X-ray powder diffraction analysis of a silver(I) cyclamate complex

X-ray powder diffraction data collected for the complex silver(I) cyclamate [Ag(C6H12NO3S)] are reported. This material was obtained from a stoichiometric mixture of sodium cyclamate and AgNO3. The analysis of the data using the Le Bail method showed that the complex has monoclinic symmetry (space group C2/c). The unit cell parameters are a=31.85852(16) angstrom, b=6.25257(6) angstrom c = 8.46165(7) angstrom, and beta=95.7651(5)degrees. (C) 2007 International Centre for Diffraction Data.

Structural characteristics of silica sonogels prepared with additions of isopropyl alcohol

Wet silica gels with similar to 1.4 x 10(-3) mol SiO2/cm(3) and similar to 92 vol% liquid phase were obtained from sonohydrolysis of tetraethoxysilane (TEOS) with different additions of isopropyl alcohol ( IPA). The IPA/TEOS molar ratio R was changed from 0 to 4. Aerogels were obtained by supercritical CO2 extraction. The samples were analyzed by small-angle X-ray scattering (SAXS) and nitrogen adsorption. The wet gels exhibit mass fractal structure with fractal dimension increasing from D similar to 2.10 to D similar to 2.22, characteristic length xi decreasing from similar to 9.5 to similar to 6.9 nm, as R increases from 0 to 4, and an estimated characteristic length for the primary silica particles lower than similar to 0.3 nm. The supercritical process apparently eliminates a fraction of the porosity, increasing the mass fractal dimension and shortening the fractality domain in the mesopore region. The fundamental role of isopropyl alcohol on the structure of the resulting aerogels is to decrease the porosity and the pore mean size as R changes from pure TEOS to R = 4. A secondary structure appearing in the micropore region of the aerogels can be described as a mass/surface fractal structure, with correlated mass fractal dimension D-m similar to 2.7 and surface fractal dimension D-s similar to 2.3, as inferred from SAXS and nitrogen adsorption data.

Thermal behavior of the Cu-22.55 at.%Al alloy with small Ag additions

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