998 resultados para Cs complexation method


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Ferroelectric barium titanate thin films were produced by the polymeric precursor method. In this technique, the desired metal cations are chelated in a solution using a hydroxycarboxylic acid as the chelating agent. Barium carbonate and titanium IV isopropoxide were used as precursors for the citrate solution. Ethylene glycol and citric acid were used as polymerization/complexation agents for the process. The crystalline structure of the film annealed at 700 °C had a single perovskite phase with a tetragonal structure. The BaTiO3 film showed good P-E hysteresis loops and C-V characteristics due to the switched ferroelectric domains.

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

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The Constant Flux: Constant Sedimentation (CF:CS) and Constant Rate of Supply (CRS) of unsupported/excess Pb-210 models have been applied to a Pb-210 data set providing of eighteen sediments profiles sampled at four riverine systems occurring in Brazil, South America: Corumbatai River basin (S1=Site 1, Sao Paulo State), Atibaia River basin (S2=Site 2, Sao Paulo State), Ribeirao dos Bagres basin (S3=Site 3, Sao Paulo State) and Amazon River mouth. (S4=Site 4, Amapa State). These sites were chosen for a comparative evaluation of the performance of the CF:CS and CRS models due to their pronounced differences on the geographical location, geological context, soil composition, biodiversity, climate, rainfall, and water flow regime, among other variable aspects. However, all sediments cores exhibited a common denominator consisting on a database built from the use of the same techniques for acquiring the sediments major chemical composition (SiO2, Al2O3, Na2O, K2O, CaO, MgO, Fe2O3, MnO, P2O5, TiO2 and LOI-Loss on Ignition) and unsupported/excess 210Pb activity data. In terms of sedimentation rates, the performance of the CRS model was better than that of the CF:CS model as it yielded values more compatible with those expected from field evidences. Under the chronological point of view, the CRS model always provided ages within the permitted range of the Pb-210-method in the studied sites, whereas the CF:CS model predicted some values above 150 years. The SiO2 content decreased in accordance with the LOI increase in all cores analyzed and such inverse relationship was also tracked in the SiO2-LOI curves of historical trends. The SiO2-LOI concentration fluctuations in sites S1 and S3 also coincided with some Cu and Cr inputs in the drainage systems. (C) 2014 Elsevier Ltd. All rights reserved.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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

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Diese Arbeit beschreibt die Entwicklung, Konstruktion und Untersuchung eines Magnetometers zur exakten und präzisen Messung schwacher Magnetfelder. Diese Art von Magnetometer eignet sich zur Anwendung in physikalischen hochpräzisions Experimenten wie zum Beispiel der Suche nach dem elektrischen Dipolmomentrndes Neutrons. Die Messmethode beruht auf der gleichzeitigen Detektion der freien Spin Präzession Kern-Spin polarisierten 3He Gases durch mehrere optisch gepumpte Cäsium Magnetometer. Es wird gezeigt, dass Cäsium Magnetometer eine zuverlässige und vielseitige Methode zur Messung der 3He Larmor Frequenz und eine komfortable Alternative zur Benutzung von SQUIDs für diesen Zweck darstellen. Ein Prototyp dieses Magnetometers wurde gebaut und seine Funktion in der magnetisch abgeschirmten Messkabine der Physikalisch Technischen Bundesanstalt untersucht. Die Sensitivität des Magnetometers in Abhängigkeitrnvon der Messdauer wurde experimentell untersucht. Es wird gezeigt, dass für kurze Messperioden (< 500s) Cramér-Rao limitierte Messungen möglich sind während die Sensitivität bei längeren Messungen durch die Stabilität des angelegten Magnetfeldes limitiert ist. Messungen eines 1 muT Magnetfeldes mit einer relative Genauigkeit von besser als 5x10^(-8) in 100s werden präsentiert. Es wird gezeigt, dass die Messgenauigkeit des Magnetometers durch die Zahl der zur Detektion der 3He Spin Präzession eingesetzten Cäsium Magnetometer skaliert werden kann. Prinzipiell ist dadurch eine Anpassung der Messgenauigkeit an jegliche experimentellen Bedürfnisse möglich. Es wird eine gradiometrische Messmethode vorgestellt, die es erlaubt den Einfluss periodischerrnmagnetischer Störungen auf dieMessung zu unterdrücken. Der Zusammenhang zwischen der Sensitivität des kombinierten Magnetometers und den Betriebsparametern der Cäsium Magnetometer die zur Spin Detektion verwendet werden wird theoretisch untersucht und anwendungsspezifische Vor- und Nachteile verschiedener Betriebsartenwerden diskutiert. Diese Zusammenhänge werden in einer Formel zusammengefasst die es erlaubt, die erwartete Sensitivität des Magnetometers zu berechnen. Diese Vorhersagen befinden sich in perfekter Übereinstimmung mit den experimentellen Daten. Die intrinsische Sensitivität des Magnetometer Prototyps wird auf Basis dieser Formel theoretisch bestimmt. Ausserdem wird die erwartete Sensitivität für die Anwendung im Rahmen des Experiments der nächsten Generation zur Bestimmung des elektrischenrnDipolmoments des Neutrons am Paul Scherrer Institut abgeschätzt. Des weiteren wird eine bequeme experimentelle Methode zur Messung des Polarisationsgrades und des Rabi Flip-Winkels der 3He Kernspin Polarisation vorgestellt. Letztere Messung ist sehr wichtig für die Anwendung in hochpräzisions Experimenten.

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Using a group of structurally related cytofectins, the effects of different vehicle constituents and mixing techniques on the physical properties and biological activity of lipoplexes were systematically examined. Physical properties were examined using a combination of dye accessibility assays, centrifugation, gel electrophoresis and dynamic light scattering. Biological activity was examined using in vitro transfection. Lipoplexes were formulated using two injection vehicles commonly used for in vivo delivery (PBS pH 7.2 and 0.9% saline), and a sodium phosphate vehicle previously shown to enhance the biological activity of naked pDNA and lipoplex formulations. Phosphate was found to be unique in its effect on lipoplexes. Specifically, the accessible pDNA in lipoplexes formulated with cytofectins containing a γ-amine substitution in the headgroup was dependent on alkyl side chain length and sodium phosphate concentration, but the same effects were not observed when using cytofectins containing a β-OH headgroup substitution. The physicochemical features of the phosphate anion, which give rise to this effect in γ-amine cytofectins, were deduced using a series of phosphate analogs. The effects of the formulation vehicle on transfection were found to be cell type-dependent; however, of the formulation variables examined, the liposome/pDNA mixing method had the greatest effect on transgene expression in vitro. Thus, though predictive physical structure relationships involving the vehicle and cytofectin components of the lipoplex were uncovered, they did not extrapolate to trends in biological activity.

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The speciation of strongly chelated iron during the 22-day course of an iron enrichment experiment in the Atlantic sector of the Southern Ocean deviates strongly from ambient natural waters. Three iron additions (ferrous sulfate solution) were conducted, resulting in elevated dissolved iron concentrations (Nishioka, J., Takeda, S., de Baar, H.J.W., Croot, P.L., Boye, M., Laan, P., Timmermans, K.R., 2005, Changes in the concentration of iron in different size fractions during an iron enrichment experiment in the open Southern Ocean. Marine Chemistry, doi:10.1016/j.marchem.2004.06.040) and significant Fe(II) levels (Croot, P.L., Laan, P., Nishioka, J., Strass, V., Cisewski, B., Boye, M., Timmermans, K.R., Bellerby, R.G., Goldson, L., Nightingale, P., de Baar, H.J.W., 2005, Spatial and Temporal distribution of Fe(II) and H2O2 during EisenEx, an open ocean mescoscale iron enrichment. Marine Chemistry, doi:10.1016/j.marchem.2004.06.041). Repeated vertical profiles for dissolved (filtrate < 0.2 µm) Fe(III)-binding ligands indicated a production of chelators in the upper water column induced by iron fertilizations. Abiotic processes (chemical reactions) and an inductive biologically mediated mechanism were the likely sources of the dissolved ligands which existed either as inorganic amorphous phases and/or as strong organic chelators. Discrete analysis on ultra-filtered samples (< 200 kDa) suggested that the produced ligands would be principally colloidal in size (> 200 kDa-< 0.2 µm), as opposed to the soluble fraction (< 200 kDa) which dominated prior to the iron infusions. Yet these colloidal ligands would exist in a more transient nature than soluble ligands which may have a longer residence time. The production of dissolved Fe-chelators was generally smaller than the overall increase in dissolved iron in the surface infused mixed layer, leaving a fraction (about 13-40%) of dissolved Fe not bound by these dissolved Fe-chelators. It is suggested that this fraction would be inorganic colloids. The unexpected persistence of such high inorganic colloids concentrations above inorganic Fe-solubility limits illustrates the peculiar features of the chemical iron cycling in these waters. Obviously, the artificial about hundred-fold increase of overall Fe levels by addition of dissolved inorganic Fe(II) ions yields a major disruption of the natural physical-chemical abundances and reactivity of Fe in seawater. Hence the ensuing responses of the plankton ecosystem, while in itself significant, are not necessarily representative for a natural enrichment, for example by dry or wet deposition of aeolian dust. Ultimately, the temporal changes of the Fe(III)-binding ligand and iron concentrations were dominated by the mixing events that occurred during EISENEX, with storms leading to more than an order of magnitude dilution of the dissolved ligands and iron concentrations. This had strongest impact on the colloidal size class (> 200 kDa-< 0.2 µm) where a dramatic decrease of both the colloidal ligand and the colloidal iron levels (Nishioka, J., Takeda, S., de Baar, H.J.W., Croot, P.L., Boye, M., Laan, P., Timmermans, K.R., 2005, Changes in the concentration of iron in different size fractions during an iron enrichment experiment in the open Southern Ocean. Marine Chemistry, doi:10.1016/j.marchem.2004.06.040) was observed.

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Background: Biodiesel is a clean-burning, renewable and biodegradable diesel fuel substitute derived from animal fats and plant oils, which may play an important role in replacing diminishing fossil fuel reserves and combating climate change. Conventional biodiesel production uses soluble base catalysts, such as Na or K alkoxides, to convert oils into fuel, and as a result requires energy intensive aqueous quench cycles to isolate the biodiesel product. Results: Cs-doping nanoparticulate MgO, prepared via a novel, supercritical sol-gel method, yields a solid base catalyst with improved activity for the transesterification of pure triacylglycerides (TAGs) and olive oil. Conclusion: Here, X-ray absorption spectroscopy (XAS) is used to probe the local chemical environment of Cs atoms in order to identify the nature of the catalytically active species as CsMg(CO)(HO). © 2013 Society of Chemical Industry.

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Produced water is a major problem associated with the crude oil extraction activity. The monitoring of the levels of metals in the waste is constant and requires the use of sensitive analytical techniques. However, the determination of trace elements can often require a pre-concentration step. The objective of this study was to develop a simple and rapid analytical method for the extraction and pre-concentration based on extraction phenomenon cloud point for the determination of Cd, Pb and Tl in produced water samples by spectrometry of high resolution Absorption source continues and atomization graphite furnace. The Box Behnken design was used to obtain the optimal condition of extraction of analytes. The factors were evaluated: concentration of complexing agent (o,o-dietilditilfosfato ammonium, DDTP), the concentration of hydrochloric acid and concentration of surfactant (Triton X -114). The optimal condition obtained through extraction was: 0,6% m v-1 DDTP, HCl 0,3 mol L-1 and 0,2% m v-1 of Triton X - 114 for Pb; 0,7% m v-1 DDTP, HCl 0,8 mol L-1 and 0,2% m v-1 Triton X-114 for Cd. For Tl was evidenced that best extraction condition occurs with no DDTP, the extraction conditions were HCl 1,0 mol L-1 e 1,0% m v-1 de Triton X - 114. The limits of detection for the proposed method were 0,005 µg L-1 , 0,03 µg L-1 and 0,09 µg L-1 to Cd, Pb and Tl, Respectively. Enrichment factors Were greater than 10 times. The method was applied to the water produced in the Potiguar basin, and addition and recovery tests were performed, and values were between 81% and 120%. The precision was expressed with relative standard deviation (RSD) is less than 5%

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The determination and monitoring of metallic contaminants in water is a task that must be continuous, leading to the importance of the development, modification and optimization of analytical methodologies capab le of determining the various metal contaminants in natural environments, because, in many cases, the ava ilable instrumentation does not provide enough sensibility for the determination of trace values . In this study, a method of extraction and pre- concentration using a microemulsion system with in the Winsor II equilibrium was tested and optimized for the determination of Co, Cd, P b, Tl, Cu and Ni through the technique of high- resolution atomic absorption spectrometry using a continuum source (HR-CS AAS). The optimization of the temperature program for the graphite furnace (HR-CS AAS GF) was performed through the pyrolysis and atomization curves for the analytes Cd, Pb, Co and Tl with and without the use of different chemical modifiers. Cu and Ni we re analyzed by flame atomization (HR-CS F AAS) after pre-concentr ation, having the sample introduction system optimized for the realization of discrete sampling. Salinity and pH levels were also analyzed as influencing factors in the efficiency of the extraction. As final numbers, 6 g L -1 of Na (as NaCl) and 1% of HNO 3 (v/v) were defined. For the determination of the optimum extraction point, a centroid-simplex statistical plan was a pplied, having chosen as the optimum points of extraction for all of the analytes, the follo wing proportions: 70% aqueous phase, 10% oil phase and 20% co-surfactant/surfactant (C/S = 4). After extraction, the metals were determined and the merit figures obtained for the proposed method were: LOD 0,09, 0,01, 0,06, 0,05, 0,6 and 1,5 μg L -1 for Pb, Cd, Tl, Co, Cu and Ni, re spectively. Line ar ranges of ,1- 2,0 μg L -1 for Pb, 0,01-2,0 μg L -1 for Cd, 1,0 - 20 μg L -1 for Tl, 0,1-5,0 μg L -1 for Co, 2-200 μg L -1 and for Cu e Ni 5-200 μg L -1 were obtained. The enrichment factors obtained ranged between 6 and 19. Recovery testing with the certified sample show ed recovery values (n = 3, certified values) after extraction of 105 and 101, 100 and 104% for Pb, Cd, Cu and Ni respectively. Samples of sweet waters of lake Jiqui, saline water from Potengi river and water produced from the oil industry (PETROBRAS) were spiked and the recovery (n = 3) for the analytes were between 80 and 112% confirming th at the proposed method can be used in the extraction. The proposed method enabled the sepa ration of metals from complex matrices, and with good pre-concentration factor, consistent with the MPV (allowed limits) compared to CONAMA Resolution No. 357/2005 which regulat es the quality of fresh surface water, brackish and saline water in Brazil.