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Journal of Thermal Analysis and Calorimetry
Authors:
Camila Xavier
,
R. Candeia
,
M. Bernardi
,
S. Lima
,
E. Longo
,
C. Paskocimas
,
L. Soledade
,
A. Souza
, and
Iêda Santos

Abstract  

Magnesium and zinc ferrites have been prepared by the polymeric precursor method. The organic material decomposition was studied by thermogravimetry (TG) and differential thermal analysis (DTA). The variation of crystalline phases and particle morphology with calcination temperature were investigated using X-ray diffraction (XRD) and scanning electronic microscopy (SEM), respectively. The colors of the ferrites were evaluated using colorimetry. Magnesium ferrite crystallizes above 800°C, presenting a yellow- orange color with a reflectance peak at the 600–650 nm range, while zinc ferrite crystallizes at 600°C, with a reflectance peak between 650–700 nm, corresponding to the red-brick color.

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Journal of Thermal Analysis and Calorimetry
Authors:
Márcia Silva
,
Lydianne de O. Miranda
,
Maria Cassia-Santos
,
S. Lima
,
L. Soledade
,
E. Longo
,
C. Paskocimas
,
A. Souza
, and
Iêda Santos

Abstract  

Undoped and/or doped with 1 mol% of Co2+ Mg2TiO4 andMg2SnO4 powders were synthesized by the polymeric precursor method. The influence of the network former (Sn4+ or Ti4+) on the thermal, structural and optical properties was investigated. The recorded mass losses are due to the escape of water and adsorbed gases and to the elimination of the organic matter. Mg2TiO4 crystallizes at lower temperatures and also presents more ordered structure with a smaller unit call and having more intense green color than Mg2SnO4 has.

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Journal of Thermal Analysis and Calorimetry
Authors:
M. Dantas
,
Marta Conceição
,
V. Fernandes Jr
,
Nataly Santos
,
R. Rosenhaim
,
Aldalea Marques
,
Iêda Santos
, and
A. Souza

Abstract  

This work evaluates the thermal and kinetic behaviour of corn biodiesel obtained by the methanol and ethanol routes. As to the TG curves, in air three thermal decomposition steps are for the methanol biodiesel and two steps are for the ethanol biodiesel. These steps are related to the evaporization and/or combustion of the methyl and ethyl esters, respectively. The corn oil presented four thermal decomposition steps in air, and only one step in nitrogen. These steps were attributed to the evaporization and/or decomposition of triglycerides. The TG and DTA profiles of the biodiesel approach the mineral diesel oil ones.

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Journal of Thermal Analysis and Calorimetry
Authors:
D. Brito
,
E. Silva
,
D. Rodrigues
,
M. Machado
,
M. Silva
,
V. Simões
,
M. Carvalho
,
L. Soledade
,
Iêda Santos
, and
A. Souza

Abstract  

A silico alumino phosphate with AFI structure (SAPO-5) was prepared in a two-phase medium and characterized by XRD, followed by the addition of TEA+. The kinetics of the TEA+/SAPO-5 thermal decomposition reaction was studied by isothermal and dynamic thermogravimetry. Two kinetic models, D3 and D4 based on diffusion processes were found as best to fit the isothermal data. On the other hand, the best fit for the dynamic data is the F1 first order reaction model. According to the apparent activation energy values, the use of the dynamic method indicates a higher temperature dependence than the isothermal method.

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Journal of Thermal Analysis and Calorimetry
Authors:
N. Santos
,
J. Santos
,
F. Sinfrônio
,
T. Bicudo
,
I. Santos
,
N. Antoniosi Filho
,
V. Fernandes
, and
A. Souza

Abstract  

The babassu (Orbignya Phalerata Mart.) biodiesel has lauric esters as main constituents, resulting in high oxidative stability and low cloud and freezing points. In order to reduce these side effects, the saturated ethyl esters content was reduced by means of winterization process. The TMDSC and PDSC techniques were used to verify the thermal and oxidative stabilities of the ethyl babassu biodiesel. During the heating stage, the winterized solid phase of ethyl esters presented an endothermic transition associated to the solidification process. This behavior was not observed for the liquid winterized FAEE, confirming the efficiency of the winterization process.

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Journal of Thermal Analysis and Calorimetry
Authors:
Rosiane M. C. Farias
,
Marta M. Conceição
,
Roberlúcia A. Candeia
,
Marta C. D. Silva
,
Valter J. Fernandes Jr.
, and
Antonio G. Souza

Abstract

The diversity of raw materials and technological routes employed in the biodiesel production has resulted in products with different chemical properties. This non-uniformity in the biodiesel composition may influence to the fuel quality. The aim of this study was to evaluate biodiesel blends of passion fruit and castor oil in different proportions and their thermal stability. Biodiesel blends of passion fruit and castor oil presented parameters in the standards of the Petroleum, Natural Gas and Biofuels National Agency. The TG curves indicated that castor oil biodiesel was more stable. Passion fruit biodiesel has a high content of oleic and linoleic acids, which are more susceptible to oxidation. Biodiesel blend of passion fruit and castor oil 1:1 increased the thermal stability in relation to passion fruit biodiesel. Biodiesel blend of passion fruit and castor oil 1:2 presented higher thermal stability, because castor oil has a high content of ricinoleic acid.

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Journal of Thermal Analysis and Calorimetry
Authors:
D. Gouveia
,
A. Souza
,
M. de Maurera
,
C. da Costa
,
I. Santos
,
S. Prasad
,
J. de Lima
,
C. Paskocimas
, and
E. Longo

Abstract  

Using the Pechini method, pigments with spinel structure (Zn7Sb2O12)were synthesized by substitution of the cation Zn2+ by Co2+, in compounds with different concentrations of Sb2O3. The doping resulted in CoxZn(7–x)Sb2O12 phases(x=1–7) that were isomorphs to spinel, denominated as samples A and B. After thermal treatment at 400C for 1 h, the powders were characterized by thermogravimetry(TG) and differential thermal analysis (DTA). The results indicate a different behavior whena higher amount of Sb2O3 is used, due to the presence of a secondary phase (ilmenite).

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Journal of Thermal Analysis and Calorimetry
Authors:
A. Garrido Pedrosa
,
M. Câmara
,
F. Borges
,
H. de Souza
,
H. Scatena Jr
,
D. Melo
, and
L. Zinner

Abstract  

Complexes of rare earth trifluoroacetates (TFA) with 4-methylmorpholine-N-oxide (MMNO) of composition Ln(TFA)33MMNO (Ln=Eu, Dy, Ho, Er, Yb and Y) were synthesized and characterized by elemental analysis data, complexometric titration with EDTA, IR absorption spectra, thermogravimetric analyses and differential scanning calorimetry (DSC) in N2 atmosphere. Infrared spectroscopy data revealed that the MMNO molecules are bound to the central ion through the oxygen of NO groups. These data suggest that the trifluoracetate groups are also coordinated. Thermogravimetric curves indicate that the decomposition of MMNO begins at approximately 350 K and results in Ln2O3 residue at around 1170 K. A theoretical kinetic study was carried out using a QBASIC program with the TG input data for the Dy complex.

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Abstract  

With the aim of obtaining materials with applications in pigments, CoxZn7-xSb2O12 spinels were synthesized using the Pechini method. This method consists in the formation of a polymeric net, where the metallic cations are homogeneously distributed. In this work, two types of alcohol (ethyl glycol and ethylene glycol) were used for the synthesis of a zinc antimoniate spinel, CoxZn7-xSb2O12 (x=0-7). The materials were characterized by termogravimetry (TG) and differential thermal analysis (DTA). TG results indicated a decrease in total mass loss when cobalt was added to the solution substituting zinc, for samples prepared using the two different alcohols. Decomposition temperatures, obtained by TG and DTA, presented a decreasing behavior as cobalt was added to the material. In relation to the alcohols, all results indicated a better polymerization of the resin when ethylene glycol was used, being the most indicated one for cation immobilization. X-ray diffraction did not show differences between the two alcohols - both presented the spinel phase (Co, Zn)2.33Sb0.67O4. Samples with higher quantity of cobalt also presented ilmenite phase (Co, Zn)Sb2O6.

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Journal of Thermal Analysis and Calorimetry
Authors:
D. Melo
,
G. Vicentini
,
L. Zinner
,
K. Zinner
,
H. de Souza
,
M. Batista
,
A. Garrido Pedrosa
, and
R. Bezerra

Abstract  

Complexes of neodymium and europium with amides and aminoxides were synthesized and characterized by complexometric analyses with EDTA, CHN microanalytical procedures, IR absorption spectra, absorption spectra of neodymium complexes, emission spectrum of europium compounds at 77 K, thermogravimetric analyses in N2 and differential scanning calorimetry (DSC) in N2. Infrared spectroscopy results revealed that the nitrate molecules are bound to the central ions as bidentate. Thermogravimetric plots indicated that the decomposition of the complexes occurs in the range 363-1163 K and resulted in the formation of Ln2O3 residues.

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