Thermal studies on nickel(II) 4-iodopyrazole complexes

This work describes the synthesis, IR and UV-Vis spectroscopic characterization as well the thermal behavior of the [NiCl2(HIPz)(4)]center dot C3H6O (1), [Ni(H2O)(2)(HIPz)(4)](NO3)(2) (2), [Ni(NCS)(2)(HIPz)(4)] (3) and [Ni(N-3)(2)(HIPz)(4)] (4) (HIPz = 4-iodopyrazole) pyrazolyl complexes. TG experiments reveal that the compounds 1-4 undergo thermal decomposition in three or four mass loss steps yielding NiO as final residue, which was identified by X-ray powder diffraction.

Anelastic relaxation processes due oxygen in Nb-3.1 at.% Ti alloys

In the last 50 years several studies have been made to understand the relaxation mechanisms of the heavy interstitial atoms present in transition metals and their alloys. Internal friction measurements have been carried out in a Nb-Ti alloy containing 3.1 at.% of Ti produced by the Materials Department of Chemical Engineering Faculty of Lorena (Brazil), with several quantities of oxygen in solid solution using a torsion pendulum. These measurements have been performed by a torsion pendulum in the temperature range from 300 to 700 K with an oscillation frequency between 0.5 and 10 Hz. The experimental results show complex internal friction spectra that have been resolved, into a series of Debye peaks corresponding to different interactions. For each relaxation process it was possible to obtain the height and temperature of the peak, the activation energy and the relaxation time of the process. (C) 2003 Elsevier B.V. All rights reserved.

Characterization of nickel doped Zn7Sb2O12 spinel phase using Rietveld refinement

Zn7Sb2O12 is known to adopt an inverse spinel crystal structure, in which Zn2+ occupies the eight tetrahedral positions and Sb5+ and Zn2+ randomly occupy the 16 octahedral positions. Samples of Zn7-xNixSb2O12 (X = 0, 1, 2, 3, and 4) were synthesized using a modified polymeric precursor method, known as the Pechini method. The crystal structure of the powders was characterized by Rietveld refinement with X-ray diffraction data. The results show that for X = 0, 1, and 2 Ni substitutes for Zn2+ in the octahedral sites, and that for X = 3 and 4 it is assumed that Ni2+ replaces Zn2+ ions in both the octahedral and tetrahedral positions. It is also observed for x = 3 and 4 the formation of two spinel phases. (C) 2003 International Centre for Diffraction Data.

Highly selective nickel ethylene oligomerization catalysts based on sterically hindered tris(pyrazolyl)borate ligands

The reaction of TlTp' (Tp' = HB(3-mesitylpyrazolyl)(3)(-) (Tp(Ms)), HB(3-mesitylpyrazolyl)(2)(5-mesitylpyrazolyl)(-) (Tp(Ms)*)) with NiCl(2).6H(2)O affords Tp(Ms)NiCl (1) and Tp(Ms)*NiCl (2) in good yield. The compound 2 undergoes an isomerization process to form [{Tp(Ms)**}NiCl](2) (3) (Tp(Ms)** = HB(5-mesitylpyrazolyl)(2)(3-mesitylpyrazolyl)(-)) in 68% yield. Treatment of the tris(pyrazolyl)-borate nickel compounds 1 and 2 with alkylaluminum cocatalysts such as methylalumoxane (MAO) and trimethylaluminum (TMA) in toluene generates active catalysts for ethylene oligomerization. The compound 1 shows turnover frequencies in the range of (2.2-43.1) x 10(3) h(-1). Oligomerization reaction conditions can be adjusted that lead to selectivities as high as 81% for butene-1.

Thermal behavior of alpha-(Cu-Al-Ag) alloys

Thermal behavior of alpha-(Cu-Al-Ag) alloys, i.e. alloys with composition less than about 8.5 mass% Al, was studied using differential scanning calorimetry (DSC), differential thermal analysis (DTA), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffractometry (XRD). The results indicated that the presence of silver introduces new thermal events ascribed to the formation of a silver-rich phase and, after addition higher amounts than 8 mass% Ag to the Cu-8 mass% Al alloy it is possible to observe the formation of the gamma(1) phase (Al4Cu9), which is only observed in alloys containing minimum of 9 mass% Al. These results may be attributed to some Ag characteristics and its interaction with Cu and Al.

Preparation of Fe-Cr-P-Co amorphous alloys by electrodeposition

The effects of bath composition and electroplating conditions on structure, morphology, and composition of amorphous Fe-Cr-P-Co deposits on AISI 1020 steel substrate, priorly plated with a thin Cu deposit, were investigated. The increase of charge density activates the inclusion of Cr in the deposit. However, above specific values of the charge density, which depend on the deposition current density, the Cr content in the deposit decreases. This Cr content decreasing is probably due to the significant hydrogen evolution with the increasing of deposition cur-rent and charge density. The effect of charge density on the content of Fe and Co is not clear. However, there is a tendency of increasing of Fe content and decreasing of Co content with the raising of current density. The Co is more easily deposited than the P, and its presence results in a more intense inhibition effect on the Cr deposition than the inhibition effect caused by P presence. Scanning electron microscope (SEM) analysis showed that Co increasing in the Fe-Cr-P-Co alloys analyzed does not promote the susceptibility to microcracks, which led to a good quality deposit. The passive film of the Fe-Cr-P-Co alloy shows a high ability formation and high protective capacity, and the results obtained by current density of corrosion, j(cor), show that the deposit with addition of Co, Fe31Cr11P28Co30, presents a higher corrosion resistance than the deposit with addition of Ni, Fe54Cr21P20Ni5. (C) 2004 Published by Elsevier B.V.

Stress-induced ordering due heavy interstitial atoms in Nb-0.3 wt.% Ti alloys

The mechanical properties of metals with bee structure, such as niobium and their alloys, are changed of a significant way by the introduction of heavy interstitial elements. These interstitial elements (oxygen, for example) present in the metallic matrix occupy octahedral sites and constitute an elastic dipole of tetragonal symmetry and might produce anelastic relaxation. Polycrystalline samples of Nb-0.3 wt.% Ti (Nb-Ti) alloy with oxygen in solid solution were analysed. The anelastic spectroscopy measurements had been made in a torsion pendulum, with frequencies in the Hz range, in a temperature range between 300 and 700 K. The results showed thermally activated relaxation structures were identified four relaxation process attributed to stress-induced ordering of single oxygen, nitrogen and carbon atoms around niobium and stress-induced ordering of single oxygen atoms around titanium atoms. (c) 2005 Elsevier B.V. All rights reserved.

Effect of Ag concentration on the thermal behavior of the Cu-10 mass% Al and Cu-11 mass% Al alloys

In this work the effect of Ag concentration on the thermal behavior of the Cu-10 mass% Al and Cu-11 mass% Al alloys with additions of 4, 6, 8 and 10 mass% Ag was studied using differential scanning calorimetry (DSC), in situ X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The results showed that for the Cu-10 mass% Al alloy Ag addition induce the beta'(1) phase formation and for the Cu-11 mass% Al alloy these additions increase the amount of martensite formed on quenching and decrease the stability range of this phase on heating.

Completeness of beta-phase decomposition reaction in Cu-Al-Ag alloys

The completeness of beta-phase decomposition reaction in the Cu-11wt%Al-xwt%Ag alloys (x = 0, 1, 2, and 3) was studied using differential scanning calorimetry (DSC), X-ray diffractometry (XRD), and optical microscopy (OM). The results indicated that beta-phase transformations are highly dependent on cooling rate and on the presence of Ag. on slow cooling, the silver presence prevents the beta- and beta(1)-phase decomposition; thus, inducing the martensitic phase formation. After rapid cooling, a new thermal event is observed and the reverse martensitic transformation is shifted to lower temperatures.

A Simple Method Based on ICP-MS for Estimation of Background Levels of Arsenic, Cadmium, Copper, Manganese, Nickel, Lead, and Selenium in Blood of the Brazilian Population

Throughout the world, biomonitoring has become the standard for assessing exposure of individuals to toxic elements as well as for responding to serious environmental public health problems. However, extensive biomonitoring surveys require rapid and simple analytical methods. Thus, a simple and high-throughput method is proposed for the determination of arsenic (As), cadmium (Cd), copper (Cu), manganese (Mn), nickel (Ni), lead (Pb), and selenium (Se) in blood samples by using inductively coupled plasma-mass spectrometry (ICP-MS). Prior to analysis, 200 l of blood samples was mixed with 500 l of 10% v/v tetramethylammonium hydroxide (TMAH) solution, incubated for 10 min, and subsequently diluted to 10 ml with a solution containing 0.05% w/v ethylenediamine tetraacetic acid (EDTA) + 0.005% v/v Triton X-100. After that, samples were directly analyzed by ICP-MS (ELAN DRC II). Rhodium was selected as an internal standard with matrix-matching calibration. Method detection limits were 0.08, 0.04, 0.5, 0.09, 0.12, 0.04, and 0.1 g//L for As, Cd, Cu, Mn, Ni, Pb, and Se, respectively. Validation data are provided based on the analysis of blood samples from the trace elements inter-\comparison program operated by the Institut National de Sante Publique du Quebec, Canada. Additional validation was provided by the analysis of human blood samples by the proposed method and by using electrothermal atomic absorption spectrometry (ETAAS). The method was subsequently applied for the estimation of background metal blood values in the Brazilian population. In general, the mean concentrations of As, Cd, Cu, Mn, Ni, Pb, and Se in blood were 1.1, 0.4, 890, 9.6, 2.1, 65.4, and 89.3 g/L, respectively, and are in agreement with other global populations. Influences of age, gender, smoking habits, alcohol consumption, and geographical variation on the values were also considered. Smoking habits influenced the levels of Cd in blood. The levels of Cu, Mn, and Pb were significantly correlated with gender, whereas Cu and Pb were significantly correlated with age. There were also interesting differences in Mn and Se levels in the population living in the north of Brazil compared to the south.

Formation of beta-nickel hydroxide plate-like structures under mild conditions and their optical properties

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Influence of doping on the preferential growth of alpha-MoO3

MoO3 is a lamellar material with applications in different areas, as solid lubricants, catalysis, solar cells, etc. In the present work, MoO3 powders, synthesized by the polymeric precursor method, were doped with nickel or cobalt. The powder precursors were characterized by TG/DTA. After calcination between 500 and 700 degrees C, the samples were characterized by X-ray diffraction, infrared and Raman spectroscopy and scanning electron microscopy. beta-MoO3 was obtained after calcination at low temperatures. With the temperature increase, alpha-MoO3 is observed, with a preferential growth of the (0 2k 0) planes, when the material is doped and calcined at 700 degrees C. Doping with nickel increases five times the preferential growth. As a consequence, plate-like particles are observed. (c) 2007 Elsevier B.V. All rights reserved.