Synthesis, characterization and thermal behavior of complexes of Cu(II), Zn(II) and Cd(II) with S,S '-methylenebis(cysteine)

Synthesis and characterization, including data on thermal decomposition, are reported for the complexes of S,S'-methylenebis(cysteine) (djenkolic acid) with copper(II), zinc(II) and cadmium(II): CuC(7)H(12)N(2)O(4)S(2) [I]; ZnC(7)H(12)N(2)O(4)S(2) [II] and CdC(7)H(12)N(2)O(4)S(2) [III] X-ray diffraction showed that the compounds are isostructural and belong to a monoclinic system. According to IR spectra, COO, NH(2) groups and bridging sulfur atoms are the main coordination sites.

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.

Arsenic as internal standard to correct for interferences in the determination of antimony by hydride generation in situ trapping graphite furnace atomic absorption spectrometry

The feasibility of using internal standardization (IS) to correct for interferences in hydride generation with in situ trapping in graphite furnace was evaluated. Arsenic was chosen as internal standard for Sb determination and Ir was used as permanent modifier. Fluctuations in the main parameters that affect the analytical results were minimized by IS and an effective contribution was verified in the studies of liquid phase interferences. Cobalt and Ni2+ were selected to illustrate the potential use of IS on the correction of interference by transition metals. The application of IS allows the Sb determination in samples containing up to 20-fold higher concentration of the Co2+ and Ni2+ when compared to the procedure without IS. The relative standard deviation of measurements varied from 0.3% to 0.7% and from 1.1% to 3.2% with and without IS, respectively. Recoveries within 92% and 107% of spiked aqueous solution containing Sb(III) and Sb(V) were found. (c) 2005 Elsevier B.V. All rights reserved.

Anelastic relaxation due to OH pairs in NbZr alloys

In the last 30 years several studies have been made to understand the relaxation mechanisms of the hydrogen atoms present in transition metals and their alloys. In this work, we observed the stress-induced ordering of hydrogen atoms around the interstitial oxygen atoms near the niobium matrix atoms. We studied this relaxation process by measuring the attenuation of longitudinal ultrasonic waves. These measurements were made in Nb1.0%Zr polycrystalline alloys at 10 and 30 MHz, pure and doped with 0.7 and 4.2 at.% hydrogen. The results revealed a thermally activated relaxation structure around 202 K and 235 K for 10 MHz and 30 MHz respectively. This relaxation structure increases with increasing hydrogen concentration. © 1994.

Microstructural development of ZnO varistor during reactive liquid phase sintering

The microstructural evolution, grain growth and densification for the varistor systems ZnO-Bi2O3 (ZB), ZnO-Bi2O3-Sb2O3 (ZBS), ZnO-Bi2O3-Sb2O3-MnO-Cr 2O3-CoO (ZBSCCM) were studied using constant heating rate sintering, scanning electron microscopy (SEM) and in situ phase formation measurement by high temperature X-ray diffraction (HT-XRD). The results showed that the densifying process is controlled by the formation and decomposition of the Zn2Bi3Sb3O14 pyrochlore (PY) phase for the ZBS and ZBSCCM systems. The addition of transition metals (ZBSCCM system) alters the formation and decomposition reaction temperatures of the pyrochlore phase and the morphology of the Zn7Sb2O12 spinel phase. Thus, the spinel grains act as inclusions and decrease the ZnO grain growth rate. Spinel grain growth kinetics in the ZBSCCM system showed an n value of 2.6, and SEM and HT-XRD results indicate two grain growth mechanisms based on coalescence and Ostwald ripening. © 1996 Chapman & Hall.

Growth parameters and nutrient content in four multipurpose tree species with potential characteristics for agroforestry systems in a Cerrado region in Botucatu, São Paulo State, Brazil

In order to evaluate growth characteristics, adaptability, biomass production, nutrient recycling, nutrient distribution and the ability to regenerate degraded land, a trial using four multipurpose tree species (Leucaena leucocephala, Leucaena diversifolia, Acacia melanoxylon and Mimosa scabrella) was undertaken over two years in a distrophic red yellow latosol (oxisol) following a randomized block experimental design with four replications. At the age of two years, A. melanoxylon and L. diversifolia were the tallest species (5.25 and 4.97 m, respectively) and A. melanoxylon and M. scabrella had the largest diameters at 20 cm from tree base. Mimosa scabrella and A. melanoxylon had the highest dry matter production and quantity of nutrients in the above ground biomass. In all species, the highest nutrient contents were found in the leaves, followed by branches and stems. From all species, the highest Nutrient Utilization Efficiency Indexes were obtained for sulphur, phosphorous, and magnesium; L. diversifolia was the most efficient for nitrogen, potassium, calcium, sulphur, and manganese, while A. melanoxylon was the most efficient for phosphorus, magnesium, boron, iron, and zinc. Litter production levels over a three month period were as follows: M. scabrella > A. melanoxylon > L. diversifolia > L. leucocephala. Litter nutrient content was higher in M. scabrella than in the other species.

Production and heat treatment of cast graphitic steels with additions of niobium

The optimal combination of the mechanical characteristics of austempered spheroidal graphitic cast steel together with modern casting techniques yielded an economically promising product. The maximum potential of the usage of these steels is related to fabrication and characterization techniques, among which, one of the most important is the cooling diagram (TTT curve). In this work, 3 heats of graphitic steels with the following nominal compositions were cast: 1.0 % C, 2.3 % Si, 0.4 % Mn, and with niobium contents of. 0.0 %, 0.5 % and 1.0 %. TTT curves were determined by dilatometric testing and test specimens of these steels were austempered. The samples were then characterized by hardness testing and optical and SEM microscopy. Tensile, impact (no notch) and wear testing were also performed. The addition of niobium produced significant alterations in the TTT diagrams. Increasing niobium content moves the pearlite transformation nose to the right and the bainitic transformation nose to the left. Tensile strength of these alloys was high, in the range of 1700 MPa and impact values were around of 45 Joules for alloy with 1 % Nb, 49 Joules for alloy with 0.5 % Nb and fracture did not occur for the alloy without the addition of Nb.

High-yield direct synthesis of Mg 2FeH 6 from the elements by reactive milling

Magnesium complex hydrides as Mg 2FeH 6 are interesting phases for hydrogen storage in the solid state, mainly due to its high gravimetric and volumetric densities of H2. However, the synthesis of this hydride is not trivial because the intermetallic phase Mg2Fe does not exist and Mg and Fe are virtually immiscible under equilibrium conditions. In this study, we have systematically studied the influence of the most important processing parameters in reactive milling under hydrogen (RM) for Mg 2FeH 6 synthesis: milling time, ball-to-powder weight ratio (BPR), hydrogen pressure and type of mill. Low cost 2Mg-Fe mixtures were used as raw materials. An important control of the Mg 2FeH 6 direct synthesis by RM was attained. In optimized combinations of the processing parameters, very high proportions of the complex hydride could be obtained. © (2011) Trans Tech Publications.

Study of adsorption and preconcentration by using a new silica organomodified with [3-(2,2′-dipyridylamine)propyl] groups

In this work, a silica surface chemically modified with [3-(2,2′-dipyridylamine)propyl] groups, named [3-(2,2′- dipyridylamine)propyl]silica (Si-Pr-DPA) was prepared, characterized, and evaluated for its heavy metal adsorption characteristics from aqueous solution. To our knowledge, we are the first authors who have reported the present modification. The material was characterized using infrared spectroscopy, SEM, and NMR 29Si and 13C solid state. Batch and column experiments were conducted to investigate for heavy metal removal from dilute aqueous solution by sorption onto Si-Pr-DPA. From a number of studies the affinity of various metal ions for the Si-Pr-DPA sorbent was determined to follow the order Fe(III) > Cr(III) >> Cu(II) > Cd(II) > Pb(II) > Ni(II). Two standard reference materials were used for checking the accuracy and precision of the method. The proposed method was successfully applied to the analysis of environmental samples. This ligand material has great advantage for adsorption of transition-metal ions from aqueous medium due to its high degree of organofunctionalization associated with the large adsorption capacity, reutilization possibility, and rapidity in reaching the equilibrium. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Adsorption of heavy metal ions and epoxidation catalysis using a new polyhedral oligomeric silsesquioxane

The objective of this research was the preparation of a silsesquioxane functionalized with eight chloropropyl chains (T8-PrCl) and of a new derivative functionalized with a pendant linear chain (2-amino-1,3,4-thiadiazole - ATD; T8-Pr-ATD). The two nanostructured materials were characterized by 13C and 29Si NMR, FTIR and elemental analysis. The new nanostructured material, octakis[3-(2-amino-1,3,4-thiadiazole)propyl] octasilsesquioxane (T8-Pr-ATD), was tested as a ligand for transition-metal ions with a special attention to adsorption isotherms. The adsorption was performed using a batchwise process and the organofunctionalized surface showed the ability to adsorb the metal ions Cu (II), Co (II), and Ni (II) from water and ethanol. The adsorption isotherms were fitted by Langmuir, Freundlich, Temkin and Dubinin-Radushkevich (D-R) model. The kinetics of adsorption of metals were performed using three models such as pseudo-first order, pseudo-second order and Elovich. The Langmuir and Elovich models were the most appropriate to describe the adsorption and kinetic data, respectively. Furthermore, the T8-Pr-ATD was successfully applied to the analysis of environmental samples (river and sea water). Subsequently, a new nanomaterial was prepared by functionalization of the T8-Pr-ATD with a Mo (II) organometallic complex (T8-Pr-ATD-Mo). Only a few works in the literature have reported this type of substitution, and none dealt with ATD and Mo (II) complexes. The new Mo-silsesquioxane organometallic nanomaterial was tested as precursor in the epoxidation of cyclooctene and styrene. © 2012 Elsevier B.V.

Sonochemical synthesis and magnetism in co-doped ZnO nanoparticles

The understanding and control of ferromagnetism in diluted magnetic semiconducting oxides (DMO) is a special challenge in solid-state physics and materials science due to its impact in magneto-optical devices and spintronics. Several studies and mechanisms have been proposed to explain intrinsic ferromagnetism in DMO compounds since the theoretical prediction of room-temperature ferromagnetism. However, genuine and intrinsic ferromagnetism in 3d-transition metal-doped n-type ZnO semiconductors is still a controversial issue. Furthermore, for DMO nanoparticles, some special physical and chemical effects may also play a role. In this contribution, structural and magnetic properties of sonochemically prepared cobalt-doped ZnO nanoparticles were investigated. A set of ZnO samples was prepared varying cobalt molar concentration and time of ultrasonic exposure. The obtained results showed that single phase samples can be obtained by the sonochemical method. However, cobalt nanoclusters can be detected depending on synthesis conditions. Magnetic measurements indicated a possible ferromagnetic response, associated to defects and cobalt substitutions at the zinc site by cobalt. However, ferromagnetism is depleted at higher magnetic fields. Also, an antiferromagnetic response is detected due to cobalt oxide cluster at high cobalt molar concentrations. © 2012 Springer Science+Business Media, LLC.

Estudo da eletrocatálise da reação de oxidação de etanol sobre fases intermetálicas ordenadas Pt-M (M = Mn,Mo, Pb, Sb e Sn)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Efeito fotocrômico em Ormosil's dopados com molibdênio preparados por síntese de Sol-Gel

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese, caracterização e estudo termoanalítico dos succinatos de alguns metais de transição bivalentes no estado sólido

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estudo de filmes poliméricos de complexos a base de tiofeno8Schiff na construção de sensores eletroquímicos

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