238 resultados para thermal drift of magnification


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

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In this present work, barium ion was reacted with different ligands which are 5,7-dibromo, 5,7-dichloro, 7-iodo and 5-chloro-7-iodo-8-hydroxyquinoline, in acetone/ammonium hydroxide medium under constant stirring and the obtained compounds were as follows: (I) Ba[(C9H4ONBr2)(2)].1.5H(2)O; (II) Ba[(C9H4ONCl2)(OH)]. 1H(2)O; (III) Ba[(C9H5ONI)(2)]. 1H(2)O and (IV) Ba[(C9H4ONICl)(2)]. 5H(2)O, respectively. The compounds were characterized by elemental analysis, infrared absorption spectrum (IR), inductively coupled plasma spectrometry (ICP), simultaneous thermogravimetry-differential thermal analysis (TG-DTA) and differential scanning calorimeter (DSC).The final residue of the thermal decomposition was characterized as orthorhombic BaBr2 from (I); the intermediate residue, as a mixture of orthorhombic BaCO3 and BaCl2 and cubic BaO and the final residue, as a mixture of cubic and tetragonal BaO and orthorhombic BaCl2 (II); the intermediate residue, as orthorhombic BaCO3 and as a final residue, a mixture of cubic and tetragonal BaO from (III); and the intermediate residue, as a mixture of orthorhombic BaCO3 and BaCl2 and as a final residue, a mixture of cubic and tetragonal BaO and orthorhombic BaCl2 from (IV).

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Pseudohalide complexes of copper(II) with aliphatic bidentate amines, [Cu(N-3)(2)(N,N-diEten)](2) 1, [Cu(NCO)(2)(N,N-diEten)](2) 2, [Cu(NCO)(2)(N,N-diMeen)](2) 3, [Cu(N-3)(NCS)(N,N'-diMeen)](2) 4 and [Cu(N-3)(NCO)(N,N-diMeen)](2) 5 (N,N-diEten=N,N-diethylethylenediamine; N,N-diMeen=N,N- dimethyl-ethylenediamine and N,N'-diMeen = N,N'-dimethylethylenediamine), were prepared, characterized and their thermal behavior was investigated by TG curves. According to thermal analysis and X-ray diffraction patterns all compounds decomposed giving copper(II) oxide as final product. The mechanisms of decomposition were proposed and an order of thermal stability was established.

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An application of photoacoustic technique is developed for determining the thermal diffusivity coefficient and the thermal conductivity of transparent materials. The backing material which supports the sample is made optically opaque, i.e., it entirely absorbs the incident light, and the converted heat diffuses through the sample heating the gas in contact with its opposite surface. The method is illustrated by fitting voltage amplitude and phase signals versus the chopping frequency in the photoacoustic cell, according to a theoretical model of heat diffusion. Thermal parameters obtained for three polymers compare very well with results from the literature. (C) 1995 American Institute of Physics.

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The influence of sample preparation strategy of vegetables on the electrothermal behaviour of Se without and with chemical modifiers such as Pd(NO3)(2), Pd(NO3)(2) + Mg(NO3)(2), Pd(NO3)(2) + Cd(NO3)(2), pre-reduced Pd, Mg(NO3)(2), and Ni(NO3)(2) was investigated. Acid digestates and slurries of vegetables (0.1% m/v in 1% m/v HNO3 + 0.005% v/v of Triton X-100) were used to prepare reference solutions or slurries. For 10 mul of each modifier tested, pyrolysis and atomization temperatures were evaluated using pyrolysis and atomization curves, respectively. Best conditions, such as thermal stability, signal profile, repeatability and sensitivity were attained using Pd(NO3)(2) as chemical modifier. The following heating program (temperature, ramp/hold time) of the graphite tube of the Varian SpectrAA-800Z atomic absorption spectrometer was used: dry step (85 degreesC, 5/0 s; 95 degreesC, 40/0 s; 120 degreesC, 10/.5 s); pyrolysis step (1400 degreesC, 10/3s); atomization step (2200 degreesC, 1/2 s); clean step (2600 degreesC, 2/0 s). This pyrolysis temperature is 800 degreesC higher than when measuring without any modifier. For 20 muL sample volume and 10 mug Pd(NO3)(2), analytical curves in the 3.0-30 mug Se 1(-1) range were obtained. The method was applied for Se determination in acid digestates and slurries of 10 vegetable samples and one standard reference material (rice flower) and results were in agreement at 95% confidence level. Recoveries varied from 89 to 95% for spiked samples. The lifetime of the graphite tube was ca. 250 firings and the relative standard deviations (n = 12) for a typical acid digestate and slurry containing 20 mug Se 1(-1) were 3.8% and 8.3%, respectively. The limits of detection were 2.0 mug Se 1(-1) and 0.6 mug Se 1(-1) Se for digestates and slurries, respectively. (C) 2002 Elsevier B.V. Ltd. All rights reserved.

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Crystalline PbTiO3 was obtained through the thermal decomposition of 8-hydroxyquinolinate of lead(II) and that of titanium(IV), which was monitored by TG/DTG/DTA under different atmospheric conditions and with varying heating rates. The compound was prepared from adding 8-hydroxyquinoline solution in the solution of metallic ions Pb(II):Ti(IV) (1:1) Linder constant stirring at 3degreesC, having the pH adjusted to 10. The results of these investigations show that different thermal behavior related to the precursor occurred and also the consequent formation of residues which have different crystallinities. No carbonate residues from the thermal decomposition could be determined by XRD and IR. Only PbTiO3 was observed and confirmed by DSC at 470degreesC, temperature lower than the tetragonal-cubic transition.

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The thermal behavior of the Cu-10 mass%Al and Cu-10 mass% Al-4 mass%Ag alloys was studied using classical differential thermal analysis (DTA), optical microscopy (OM) and X-ray diffractometry (XRD). The DTA curves were obtained for annealed and quenched samples. The results indicated that the presence of silver introduces new thermal events, associated to the formation of a silver-rich phase, to the shift of the equilibrium concentration to higher A1 contents and to the decomposition of the silver-rich phase in the same temperature range of the beta(1) phase decomposition.

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Solid state Ln-4-Me-BP compounds, where Ln stands for lighter trivalent lanthanides (lanthanum to europium) and 4-Me-BP is 4-methylbenzylidenepyruvate, have been synthesized. Elemental analysis, complexometry, X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA), have been used to characterize and to study the thermal behaviour of these compounds. The results provided information concerning the stoichiometry, crystallinity, thermal stability and thermal decomposition. (C) 2002 Elsevier B.V. B.V. All rights reserved.

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Steady-state concentric cylinder equipment was used to determine the effective thermal conductivity of beans (Phaseolus vulgaris). The measuring cell had no heated end guards and its length to diameter ratio was 10.5. Glass beads were employed to assess the accuracy and repeatability of the experimental system under heat transfer conditions. The results agree well with those reported in the literature so that the system can be considered reliable. Corn was used to verify the system's accuracy under heat and mass transfer conditions. Again the results were satisfactory. Moisture migration was observed and measured during the tests with beans, but this behavior does not compromise thermal conductivity values if both thermal and mass transfer steady-states are correctly interpreted. The effective thermal conductivity increases linearly with increasing grain moisture content. Statistical regression leads to good estimates of the fitted parameters.

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The thermal behavior of simple and mixed pyrazolyl complexes [PdCl2(phmPz)(2)] (1),[Pd(N-3)(2)(phmPz)(2)] (2), [Pd(SCN)(2)(phmPz)(2)] (3), and [Pd(N-3)(SCN)(phmPz)(2)] (4) (phmPz: 1-phenyl-3-methylpyrazole) has been investigated by means of thermogravimetry (TG) and differential thermal analysis (DTA). From the initial decomposition temperatures, the thermal stability of the complexes can be ordered in the sequence: 4 < 2 < 3 < 1. The final products of the thermal decompositions were characterized as metallic palladium (Pd-0). (C) 2004 Elsevier B.V. All rights reserved.

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Samples of commercial alkyd resin varnish were spread in a film form on slides, dried at room temperature and exposed to solar radiation from one day up to seven months.Thermogravimetric measurements have been done. Based on the TG data, the Flynn-Wall isoconversional method was applied. The activation energy varied between 176-154 kJ mol(-1) and logA was between 15.5-12.9 min(-1) for A, B and C samples at 95% confidence level.

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A structural study of the thermal evolution of Ni0.69Cr0.31(OH)(2)(CO3)(0.155)(.)nH(2)O into NiO and tetragonal NiCr2O4 is reported. The characteristic structural parameters of the two coexisting crystalline phases, as well as their relative abundance, were determined by Rietveld refinement of powder x-ray diffraction (PXRD) patterns. The results of the simulations allowed us to elucidate the mechanism of the demixing process of the oxides. It is demonstrated that nucleation of a metastable nickel chromite within the common oxygen framework of the parent Cr-III-doped bunsenite is the initial step of the cationic redistribution. The role that trivalent cations play in the segregation of crystalline spinels is also discussed.

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The synthesis, characterization and thermal analysis of the novel cyclometallated compounds [Pd-2(dmba)(2)Cl-2(mu-bpe)] (1), [Pd-2(dmba)(2)(N-3)(2)(mu-bpe)] (2), [Pd-2(dmba)(2)(NCO)(2)(mu-bpe)] (3), [Pd-2(dmba)(2)(SCN)(2)(mu-bpe)] (4), [Pd-2(dmba)(2)(NO3)(2)(mu-bpe)] (5) (bpe=trans-1,2-bis(4-pyridyl)ethylene; dmba=N,N-dimethylbenzylamine) are described. The thermal stability of [Pd-2(dmba)(2)X-2(mu-bpe)] complexes varies in the sequence 1 > 4 > 3 > 2 > 5. The final residues of the thermal decompositions were characterized as metallic palladium by X-ray powder diffraction.

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The freezing point depression (FPD) of orange juice at different concentrations was measured by using a simple apparatus. Results showed that the initial freezing point decreased approximately 90% with the increase of juice concentration between 46degrees and 66degrees Brix (water content respectively between 52.8 and 32.8% w/w). The thermal conductivity of orange juice as a function of fluid concentration was also investigated by using a coaxial dual-cylinder apparatus. Below the freezing point, the thermal conductivity was strongly affected by both the orange juice concentration and temperature. Simple equations in terms of water content and temperature could be adjusted to experimental data of FPD and thermal conductivity.