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Abstract  

The present work proposes evaluation of the gelatinization processes of starch by means of DSC coupled with a photovisual system. The use of DSC, TG and DTA for a fast and efficient evaluation of the starch is suggested. The DSC curves of starch gels with water contents of 20, 30, 40 and 50% (mass/v) exhibited different phase transitions, corresponding to the gelatinization processes at the different water contents for the different lots. The DSC-photovisual system confirmed calorimetric behaviour differences between the starch lots studied.

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Abstract  

The color efficiency of ceramic glaze blue pigments obtained by the Pechini method was presented in this work. The fired pigments and enameled samples were characterized by thermogravimetry (TG) and differential thermal analysis (DTA), XRD, UV-VIS-NIR spectroscopy and CIE-L*a*b* color-measurements. The pigments obtained by the Pechini method present a better solubility in the molten glazes than the pigments obtained by the mechanical mixture of the precursor oxides.

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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:
R. Macêdo
,
J. Barbosa-Filho
,
E. da Costa
, and
A. de Souza

Abstract  

The terpenoids acetyl sitosterol, lupeol, acetyl diosgenin and stigmasterol were studied. Comparison of the thermogravimetric curves and the activation energies of the terpenoids suggested the following sequence of thermal stability: acetyl sitosterol < acetyl diosgenin < lupeol < stigmasterol. The DSC curves allowed determination of the melting points and the degrees of purity. Comparison of the TG and DSC curves revealed the presence of phase transitions without mass loss that were attributed to rearrangements in the terpenoid molecules.

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Abstract  

The thermal decomposition kinetics of the solid complexes Cd(S2 CNR2 )2 , where R =C2 H5 , n -C3 H7 , n -C4 H9 or iso -C4 H9 , was studied by using isothermal and non-isothermal thermogravimetry. The superimposed TG/DTG/DSC curves revealed that thermal decomposition reactions occur in the liquid phase. The kinetic model that best fitted the experimental isothermal TG data was the one-dimensional phase-boundary reaction-controlled process R1 . The thermal analysis data suggested the thermal stability sequence Cd(S2 CNBun 2 )2 >Cd(S2 CNPrn 2 )2 >Cd(S2 CNBui 2 )2 >Cd(S2 CNEt2 )2 , which accords with the sequence of stability of the apparent activation energies.

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Abstract  

Hair analysis presents a lot of advantages compared to the analysis of biological fluids or tissues. Hair of employers from the National (Brazilian) Nuclear Energy Commission (CNEN) was analyzed and compared with a control group. Samples were heated at 90°C with nitric acid, and diluted. Aliquot of these solutions was analyzed in ICP-MS. The concentration of U, Th, Pb and Zn were determined. Student t-test showed that there is no significant difference among the groups for all analyzed elements. The results demonstrated that men had more Pb than women. For Zn, the results showed that the levels are within the “normal” range, except for a woman that had her hair painted.

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In this perspective article, the use of continuous flow synthesis to prepare advanced pharmaceutical intermediates in developing economies is highlighted. Case studies are presented to suggest that cost effective local manufacture of life saving drugs, may potentially be implemented to facilitate better access to drugs to the underprivileged.

Open access
Journal of Thermal Analysis and Calorimetry
Authors:
E. F. S. M. Ramalho
,
A. R. Albuquerque
,
A. L. Souza
,
A. K. Barro
,
A. S. Maia
,
I. M. G. Santos
, and
A. G. Souza

Abstract

The poultry fat methylic (BMF) and ethylic (BEF) biodiesels were synthesized through transesterification by homogeneous basic catalysis. The chromatographic analyses showed the palmitic, stearic, oleic, and linoleic esters as majority components. Owing to its considerable amount of polyunsaturated fat acids, poultry fat usually leads to a biodiesel with low oxidative stability. In this study, the oxidation of their ethylic and methylic biodiesels was evaluated by Rancimat, PDSC, and PetroOxy. The OSI (Rancimat) was of 0.47 and 0.40 h for the ethylic and methylic biodiesel, respectively. In PDSC, both fuels presented an OT of about 120–123 °C. PetroOxy analysis indicated an OxyStab of 11 min for BEF and higher than 11 min for BMF. There was no correspondence among the oxidative stabilities of the employed techniques [OT(BEF) ≈ OT(BMF), OSI(BEF) > OSI(BMF), and OxyStab(BEF) < OxyStab(BMF)]. The discussion of these results was based on the indicator measured by each technique: enthalpic events are observed by PDSC; conductivity of volatile secondary oxidation products is measured by Rancimat; reduction of the oxygen pressure is determined by PetroOxy. This discussion showed that these different indicators do not reflect the same stage of the oxidative process as energy is release at the beginning of the propagation step, oxygen pressure decreases during the propagation step, and oxidation products are formed during the termination step.

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Journal of Thermal Analysis and Calorimetry
Authors:
A. de Oliveira
,
J. Ferreira
,
Márcia Silva
,
Soraia de Souza
,
F. Vieira
,
E. Longo
,
A. Souza
, and
Iêda Santos

Abstract  

NiWO4 and ZnWO4 were synthesized by the polymeric precursor method at low temperatures with zinc or nickel carbonate as secondary phase. The materials were characterized by thermal analysis (TG/DTA), infrared spectroscopy, UV–Vis spectroscopy and X-ray diffraction. NiWO4 was crystalline after calcination at 350 °C/12 h while ZnWO4 only crystallized after calcination at 400 °C for 2 h. Thermal decomposition of the powder precursor of NiWO4 heat treated for 12 h had one exothermic transition, while the precursor heat treated for 24 h had one more step between 600 and 800 °C with a small mass gain. Powder precursor of ZnWO4 presented three exothermic transitions, with peak temperatures and mass losses higher than NiWO4 has indicating that nickel made carbon elimination easier.

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Journal of Thermal Analysis and Calorimetry
Authors:
Soraia de Souza
,
Mary Alves
,
A. de Oliveira
,
E. Longo
,
F. Ticiano Gomes Vieira
,
Rodinei Gomes
,
L. Soledade
,
A. de Souza
, and
Iêda Garcia dos Santos

Abstract  

In this work, the synthesis of Nd-doped SrSnO3 by the polymeric precursor method, with calcination between 250 and 700 °C is reported. The powder precursors were characterized by TG/DTA and high temperature X-ray diffraction (HTXRD). After heat treatment, the material was characterized by XRD and infrared spectroscopy. Ester and carbonate amounts were strictly related to Nd-doping. According to XRD patterns, the orthorhombic perovskite was obtained at 700 °C for SrSnO3 and SrSn0.99Nd0.01O3. For Sr0.99Nd0.01SnO3, the kinetics displayed an important hole in the crystallization process, as no peak was observed in HTXRD up to 700 °C, while a XRD patterns showed a crystalline material after calcination at 250 °C.

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