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Abstract  

This study focuses on the thermal and structural characteristics of some Brazilian kaolinitic clays. X-ray diffraction analysis have shown that the clay samples consist mainly of kaolinite, and quartz and gibbsite as principal impurities. On heating three endothermic transformations were identified as water loss from TG-MS data within the 60-64, 268-276 and 499-503C ranges, followed by an exothermic transformation with maximum within the 950-959C range. The endothermic valleys can be mainly interpreted as the release of free moisture, dehydration of gibbsite and dehydroxylation of kaolinite, respectively. The exothermic peak is associated with crystallization of new phases from metakaolinite. The quantification of kaolinite (59.6-74.2%) and gibbsite (5.9-10.2%) was taken by the thermogravimetric measurements. In addition, it was also demonstrated from the thermal curves that the character of the clays from South-Eastern Brazil (Campos-RJ) is predominantly kaolinic.

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Abstract  

We present the measure of quality introduced by the review team of Embrapa to evaluate its research projects. The quality measurement scheme comprises four different dimensions (External Validity, Internal Validity, Institutional Adequacy, and Formal Adequacy). The quality measurements are used as dependent variables in a multivariate effort to identify important factors necessary to improve overall as well as specific quality aspects.

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Biodiesels from beef tallow/soybean oil/babassu oil blends

Correlation between fluid dynamic properties and TMDSC data

Journal of Thermal Analysis and Calorimetry
Authors:
G. A. A. Teixeira
,
A. S. Maia
,
I. M. G. Santos
,
A. L. Souza
,
A. G. Souza
, and
N. Queiroz

Abstract

Cloud point (CP), cold filter plugging point (CFPP), and pour point (PP) of biodiesel samples obtained from blends containing different amounts of beef tallow, babassu oil, and soybean oil were investigated by the corresponding conventional techniques and by temperature modulated differential scanning calorimetry (TMDSC). The CP and CFPP values correlate well with the crystallization temperature (T onset) obtained from the TMDSC curves, being the highest for the biodiesel sample containing the highest amount of methyl stearate. A correspondence between PP and the peak temperature was also noticed, pointing out that pouring ceases after the crystallization of the heavier fatty acid ester. Among the samples of biodiesel, Bio-3 (highest amount of babassu oil) and Bio-4 (highest amount of soybean oil) showed better cold-flow properties, or in other words, lower values of CP, CFPP, and PP. Independently of the composition, the cold-flow properties of all biodiesel samples meet the requirements from the Brazilian National Agency of Petroleum, Natural Gas, and Biofuels (ANP).

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Abstract

Biodiesel can be obtained from various fatty acid sources. Each raw material has a different chemical composition that leads to different properties. Owing to these properties, the mixture of different proportions of raw materials can lead to biodiesels with best features in relation to physicochemical parameters such as viscosity, oxidative stability and flow properties, generating a fuel whose characteristics meet the requirements of the current legislation of the Brazilian National Agency of Petroleum, Natural Gas and Biofuels (ANP). The objective of this study was to determine the physicochemical properties of biodiesel samples produced from mixtures of beef tallow, babassu oil, and soybean oil. The thermo-oxidative stability was evaluated using thermogravimetry (TG/DTG) and differential scanning calorimetry (DSC). The results showed that all samples were in accordance to the ANP specifications. The biodiesel obtained from a mixture containing 50% of babassu oil had lower values of pour point, cold filter plugging point, and freezing point. This biodiesel also showed a higher thermo-oxidative stability in synthetic air and in oxygen atmospheres.

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Journal of Thermal Analysis and Calorimetry
Authors:
M. A. F. Souza
,
R. A. Candeia
,
S. J. G. Lima
,
M. R. Cassia-Santos
,
I. M. G. Santos
,
E. Longo
, and
A. G. Souza
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Solid state reactions in the platinum–mercury system

Thermogravimetry and differential scanning calorimetry

Journal of Thermal Analysis and Calorimetry
Authors:
G. Souza
,
I. Pastre
,
A. Benedetti
,
C. Ribeiro
, and
F. Fertonani

Abstract  

Thermogravimetry, Differential Scanning Calorimetry and other analytical techniques (Energy Dispersive X-ray Analysis; Scanning Electron Microscopy; Mapping Surface; X-ray Diffraction; Inductively Coupled Plasma Atomic Emission Spectroscopy and Cold Vapor Generation Atomic Absorption Spectroscopy) have been used to study the reaction of mercury with platinum foils. The results suggest that, when heated, the electrodeposited Hg film reacts with Pt to form intermetallic compounds each having a different stability, indicated by at least three mass loss steps. Intermetallic compounds such as PtHg4, PtHg and PtHg2 were characterized by XRD. These intermetallic compounds were the main products formed on the surface of the samples after partial removal of bulk mercury via thermal desorption. The Pt(Hg) solid solution formation caused great surface instability, attributed to the atomic size factor between Hg and Pt, facilitating the acid solution’s attack to the surface.

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Abstract  

Thermogravimetry (TG), cyclic voltammetry (CV) and other analytical techniques were used to study the reactions of mercury with Pt–30% Ir alloy. The results allowed to suggest that an electrodeposited mercury film interacts with the substrate and when subjected to heat or electrochemical removal at least four mass loss steps or five peaks appeared during the mercury desorption process. The first two steps were attributed to Hg(0) removal probably from the bulk and from the adsorbed monolayer which wets the electrode surface. These two processes are responsible for peaks D and F in the cyclic voltammograms. The last two peaks (G, H) in CV were ascribed to the intermetallic compound decomposition. In TG curves, the last two steps were attributed to the PtHg4 (third step), and PtHg2 decomposition followed by Hg removal from the subsurface. The PtHg2 was formed by an eutectoide reaction: PtHg→PtHg2+Hg(Pt–Ir). The Hg diffused to the subsurface was not detectable by cyclic voltammetry.

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Abstract  

Solid-state M-EDTA chelates, where M represents the divalent ions Mg(II), Ca(II), Sr(II) or Ba(II) and EDTA is ethylenediaminetetraacetate anion, were synthesized. Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC) and X-ray diffraction powder patterns have been used to characterize and to study the thermal behaviour of these chelates. The results provided information concerning the stoichiometry, crystallinity, thermal stability and thermal decomposition.

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Journal of Thermal Analysis and Calorimetry
Authors:
Adney Luís A. da Silva
,
Guilherme G. G. Castro
, and
Mariana M. V. M. Souza

Abstract

Lanthanum strontium chromite (LSC) powders were synthesized by the combustion method, using five different fuels (urea, glycine, ethylene glycol, α-alanine, and citric acid). The ignition of the reagent mixture with urea takes a longer time, and more gases are released by combustion. A calcination step is essential for a good crystallization of the perovskite phase. X-ray diffraction patterns showed formation of perovskite phase and a small amount of SrCrO4 for the sample synthesized with urea after calcination. The crystallite sizes are in the range of 23–33 nm. Scanning electron microscopy revealed the porosity of the powders and the presence of agglomerates, formed by fine particles of different shapes. Thermogravimetric analysis showed a large mass loss for the sample synthesized with citric acid, probably caused by the absence of ignition, with primary polymerization of the precursor reagents.

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Journal of Thermal Analysis and Calorimetry
Authors:
G. Fontanari
,
G. Souza
,
J. Batistuti
,
V. Neves
,
I. Pastre
, and
F. Fertonani

Abstract  

Glutelin, the major protein fraction from guava seed, was obtained by fractioning as described by Osborne. The total proteins were extracted and the isolates obtained by isoelectric precipitation presented similar DSC curves, concordant with the results obtained by gel filtration chromatography and electrophoresis in polyacrylamide gel (PAGE-SDS). However, the DSC curves showed a higher enthalpy with regard to the denaturing protein isolate (PI) extracted at pH 10.0 when compared to a PI at pH 11.5. Such results are in accordance with those obtained for PI extracted at pH 10.0 using chromatography, this one being present in the form of molecular aggregates of greater molecular mass. The glutelin fraction, however, did not present a denaturation peak in the DSC curve, showing that the process for obtaining the same significantly altered its conformation.

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