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Abstract  

The effect on the stability of the isomers of aminosalicylic acid of formation of their sodium salts has been studied by use of differential scanning calorimetry and thermogravimetry, coupled with evolved gas analysis by Fourier transform infrared spectroscopy. X-ray powder diffraction and infrared spectroscopy provided complementary information. The DSC curves for the sodium salts of all of the isomers showed complex dehydration/decomposition endotherms. From the initial mass losses of the TG curves, the amounts of water per mole of salt were estimated as 0.5, 2.4 and 1.4 moles for the sodium salts of 3-aminosalicylic acid, 4-aminosalicylic acid and 5-aminosalicylic acid, respectively. TG-FTIR results for the sodium salt of 3-aminosalicylic acid showed the evolution of carbon dioxide in three stages: below 150C, between 200 and 300C and continuous formation up to 500C. This behaviour differs from that of 3-aminosalicylic acid itself, which forms CO2 between 225 and 290C. For the sodium salt of 4-aminosalicylic acid, the formation of carbon dioxide starts from 250C and is still being formed at about 650C. 4-aminosalicylic acid decarboxylates above 150C. 5-aminosalicylic acid and its sodium salt showed no evolution of carbon dioxide below 600C.

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Abstract  

Coupled TG-FTIR technique was used for identification of gaseous compounds evolved at thermal treatment of six coal samples from different deposits (Bulgaria, Russia, Ukraine). The experiments were carried out under dynamic heating conditions up to 900C at heating rates of 5, 10 or 50 K min–1 in a stream of dry air. The emission of CO2, H2O, CO, SO2, COS, methane, methanol, formic acid, formaldehyde, acetaldehyde, chlorobenzene was clearly identified in FTIR spectra of the samples studied. The formation of ethanol, ethane, ethylene and p-xylene, at least on the level of traces, was also identified. At the heating rate of 5C min–1 the temperature of maximum intensities of the characteristic peaks of COS was 270C, of formaldehyde, formic acid, ethane and methanol 330C, of SO2, CO, acetic acid, ethylene and p-xylene 400C and of chlorobenzene 500C. At 10C min–1 and 50C min–1 these temperatures were shifted, respectively, by 70–300C and 150–450C towards higher temperatures and the respective absorption bands in FTIR spectra were, as a rule, more intensive.

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Journal of Thermal Analysis and Calorimetry
Authors:
B. Zapata
,
J. Balmaseda
,
E. Fregoso-Israel
, and
E. Torres-García

Abstract  

Thermal degradation of orange peel was studied in dynamic air atmosphere by means of simultaneous TG-DSC and TG-FTIR analysis. According to the obtained thermal profiles, the orange peel degradation occurred in at least three steps associated with its three main components (hemicellulose, cellulose and lignin). The volatiles compounds evolved out at 150–400 °C and the gas products were mainly CO2, CO, and CH4. A mixture of acids, aldehydes or ketones C=O, alkanes C–C, ethers C–O–C and H2O was also detected. The E α on α dependence reveled the existence of different and simultaneous processes suggesting that the combustion reaction is controlled by oxygen accessibility, motivated by the high evolution low-molecular-mass gases and volatile organic compounds. These results could explain the non-autocatalytic character of the reactions during the decomposition process.

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Abstract  

The thermal decomposition behaviour of the manganese(II) complexes with glycine: Mn(gly)Cl2(H2O)2, Mn(gly)2Cl2, Mn(gly)Br2(H2O)2, Mn(gly)2Br2(H2O)2 was investigated by means of TG-DTG-DTA, Hi-Res-TA and DSC techniques. The evolved gas analysis was carried out by means of the coupled TG-FTIR system. Heating of the complexes results first in the release of water molecules. Next, the multi-stage decomposition process with degradation of glycine ligand occurs. Water, carbon dioxide and ammonia were detected in the gaseous products of the complexes decomposition. The temperature of NH3 evolution from the complexes is higher than from free glycine. The final residue in the air atmosphere is Mn2O3 which transforms into Mn3O4 at 930C. In a nitrogen atmosphere, the complexes decompose into MnO.

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Abstract  

The new 1,2,4-benzenetricarboxylates of lanthanide(III) of the formula Ln(btc)�nH2O, where btc is 1,2,4-benzenetricarboxylate; Ln is La-Lu, and n=2 for Ce; n=3 for La, Yb, Lu; and n=4 for Pr-Tm were prepared and characterized by elemental analysis, infrared spectra and X-ray diffraction patterns. Polycrystalline complexes are isotructural in the two groups: La-Tm and Yb, Lu. IR spectra of the complexes show that all carboxylate groups from 1,2,4-benzentricarboxylate ligands are engaged in coordination of lanthanide atoms. The thermal analysis of the investigated complexes in air atmosphere was carried out by means of simultaneous TG-DTA technique. The complexes are stable up to about 30�C but further heating leads to stepwise dehydration. Next, anhydrous complexes decompose to corresponding oxides. The combined TG-FTIR technique was employed to study of decomposition pathway of the investigated complexes.

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Abstract  

The thermal decomposition of strontium acetate hemihydrate has been studied by TG-DTA/DSC and TG coupled with Fourier transform infrared spectroscopy (FTIR) under non-isothermal conditions in nitrogen gas from ambient temperature to 600°C. The TG-DTA/DSC experiments indicate the decomposition goes mainly through two steps: the dehydration and the subsequent decomposition of anhydrous strontium acetate into strontium carbonate. TG-FTIR analysis of the evolved products from the non-oxidative thermal degradation indicates mainly the release of water, acetone and carbon dioxide. The model-free isoconversional methods are employed to calculate the E a of both steps at different conversion α from 0.1 to 0.9 with increment of 0.05. The relative constant apparent E a values during dehydration (0.5<α<0.9) of strontium acetate hemihydrate and decomposition of anhydrous strontium acetate (0.5<α<0.9) suggest that the simplex reactions involved in the corresponding thermal events. The most probable kinetic models during dehydration and decomposition have been estimated by means of the master plots method.

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Rare-earth based OLEDs

TG-FTIR thermal stability investigation of tetrakis beta-diketonates complexes

Journal of Thermal Analysis and Calorimetry
Authors:
Kelly C. Teixeira
,
Gabriela F. Moreira
,
Welber G. Quirino
,
Cristiano Legnani
,
Raigna A. Silva
,
Marco Cremona
,
Hermi F. Brito
, and
Carlos A. Achete

resulting in the more stable tris-species. This does not happen for the Li[Eu(dbm) 4 ]·4H 2 O, which is thermally more stable, as the TG-FTIR measurement indicates. Conclusions The TG-FTIR results suggest that Li[Eu(dbm) 4

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Abstract  

In order to improve poly(vinyl chloride) (PVC) thermal stability, poly(vinyl butyral) (PVB) matrix and calcium carbonate nanoparticles were incorporated in plasticized PVC. Thermal properties of these composites were investigated by thermogravimetry analysis coupled with mass spectrometry and Fourier transform infrared spectroscopy (FTIR). This approach highlighted the efficiency of both PVB and CaCO3 as HCl scavengers by postponing both the onset degradation temperature and the HCl release. Moreover, a synergetic effect was evidenced regarding the HCl release. Finally, kinetic parameters of the PVC first degradation stage, determined using the Flynn–Wall–Ozawa’s method, revealed a significant increase of the activation energy by incorporation of CaCO3 in the presence or not of PVB.

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Abstract  

Thermal properties of cis-1,4-poly(butadiene), Europrene cis, were investigated by means of thermal analysis and complementary methods. Thermal analysis of polymer was carried out both in air and inert atmosphere with a derivatgraph, DSC and internal TG-FTIR coupling system as well as internal TG, DTA-MS coupling system. It was found that investigations in air atmosphere the method of the sample preparation ofcis-1,4-poly(butadiene) influences the results of thermal analysis, which is connected with the rate oxygen diffusion into the reaction zone. Taking into consideration both the method of the sample preparing and atmosphere of thermal studies, the values of activation energy of destruction of cis-1,4-poly(butadiene) were determined. Using TG-FTIR and TG-MS methods, some products of thermal destruction of elastomer were determined.

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Journal of Thermal Analysis and Calorimetry
Authors:
S. Jingyan
,
L. Jie
,
D. Yun
,
H. Ling
,
Y. Xi
,
W. Zhiyong
,
L. Yuwen
, and
W. Cunxin

Abstract  

The thermal behavior of nicotinic acid under inert conditions was investigated by TG, FTIR and TG/DSC-FTIR. The results of TG/DSC-FTIR and FTIR indicated that the thermal behavior of nicotinic acid can be divided into four stages: a solid-solid phase transition (176–198°C), the process of sublimation (198–232°C), melting (232–263°C) and evaporation (263–325°C) when experiment was performed at the heating rate of 20 K min−1. The thermal analysis kinetic calculation of the second stage (sublimation) and the fourth stage (evaporation) were carried out respectively. Heating rates of 1, 1.5, 2 and 3 K min−1 were used to determine the sublimation kinetics. The apparent activation energy, pre-exponential factor and the most probable model function were obtained by using the master plots method. The results indicated that sublimation process can be described by one-dimensional phase boundary reaction, g(α)=α. And the ‘kinetic triplet’ of evaporation process was also given at higher heating rates of 15, 20, 25, 30 and 35 K min−1. Evaporation process can be described by model of nucleation and nucleus growing,
\documentclass{aastex} \usepackage{amsbsy} \usepackage{amsfonts} \usepackage{amssymb} \usepackage{bm} \usepackage{mathrsfs} \usepackage{pifont} \usepackage{stmaryrd} \usepackage{textcomp} \usepackage{upgreek} \usepackage{portland,xspace} \usepackage{amsmath,amsxtra} \pagestyle{empty} \DeclareMathSizes{10}{9}{7}{6} \begin{document} $$g(\alpha ) = \left[ { - \ln (1 - \alpha )} \right]^{\frac{1} {3}}$$ \end{document}
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