Application to polymer characterization by thermal analysis

The measured results of thermal analysis depend on experimental conditions. The international and national organizations have constituted a series of methods to characterize the physical and chemical properties for substances. The applications to physical transition, chemical reaction, and characteristic parameters of substances are given in the article as examples.

Thermodynamic study of ibuprofen by adiabatic calorimetry and thermal analysis

Molar heat capacities of ibuprofen were precisely measured with a small sample precision automated adiabatic calorimeter over the temperature range from 80 to 400 K. The polynomial functions of C-p,C-m (J K-1 mol(-1)) versus T were established on the heat capacity measurements by means of the least fitting square method. The functions are as follows: for solid ibuprofen, at the temperature range of 79.105 K less than or equal to T less than or equal to 333.297 K, C-p,C-m = 144.27 + 77.046X + 3.5171X(2) + 10.925X(3) + 11.224X(4), where X = (T - 206.201)/127.096; for liquid ibuprofen, at the temperature range of 353.406 K less than or equal to T less than or equal to 378.785 K, C-p,C-m = 325.79 + 8.9696X - 1.6073X(2) - 1.5145 X-3, where X = (T - 366.095)/12.690. A fusion transition at T = 348.02 K was found from the C-p-T curve. The molar enthalpy and entropy of the fusion transition were determined to be 26.65 kJ mol(-1) and 76.58 J mol(-1) K-1, respectively. The thermodynamic functions on the base of the reference temperature of 298.15 K, (H-T - H-298.15) and (S-T - S-298.15), were derived. Thermal characteristic of ibuprofen was studied by thermo-gravimetric analysis (TG-DTG) and differential scanning calorimeter (DSC). The temperature of fusion, the molar enthalpy and entropy of fusion obtained by DSC were well consistent with those obtained by adiabatic calorimeter. The evaporation process of ibuprofen was investigated further by TG and DTG, and the activation energy of the evaporation process was determined to be 80.3 +/- 1.4 kJ mol(-1). (C) 2003 Elsevier B.V. All rights reserved.

Thermal analyses, spectral characterization and structural interpretation of Yb3+ doped TeO2-ZnO-ZnCl2 glasses

Bulk-lasses have been prepared in the TeO2-ZnO-ZnCl2 systems. Their characteristic temperatures were determined and analyzed. Raman and FT-IR spectra were used to analyze the effect of ZnCl2 on the structure and spectral properties of tellurite glasses and OH- groups in this glass system. The spectroscopic properties including absorption spectra, emission cross-sections and fluorescence lifetimes of Yb3+ in TeO2-ZnO-ZnCl2 were measured and calculated. It is demonstrated that the progressive replacement less than 20 mol% of TeO2 by ZnCl2 improves the thermal stability, removes the OH- groups, turns TeO4 bipyramidal arrangement into TeO3 (and/or TeO3+1) trigonal pyramids structures and results in the decrease of the symmetry of the structure, which increases the emission cross-sections and lifetimes. But when the content of ZnCl2 up to 30 mol%, the glass system becomes more hygroscopic and introduces more OH- groups, which decrease the emission cross-sections and shorten the lifetimes. The results show that the glass system with (TeO2)-Te-69-(ZnO)-Zn-10-20ZnCl(2)-1Yb(2)O(3) is a desirable component for active laser media for high power generation. (c) 2005 Elsevier B.V. All rights reserved.

Thermal analysis of glasses in TeO2-BaF2-LaF3 systems

Divalent metal fluorides MF2 (M=Sr, Mg, Ca) in oxyfluoride tellurite glasses TeO2-BaF2-LaF3 were synthesized. The densities, refractive indices and characteristic temperatures of synthesized glasses were measured. The influence of divalent metal fluorides MF2 (M=Sr, Mg, Ca) on the thermal stability of oxyfluoride tellurite glasses TeO2-BaF2-LaF3 were studied. Results show that the replacement of BaF2 by SrF2 and MgF2 can enhance the thermal stability against crystallization of the glass. A glass system with good thermal stability was produced, which could be a potential candidate for the host materials of the fiber devices.

Thermal analysis of microstructural evolution of Al2O3 surface modified layers

Solidification behavior and microstructural evolution of surface modified layers in plasma cladding technique are studied via numerical simulations. Both the coupling effect of temperature and solid volume fraction are considered in the proposed thermal analytical model, by which the transient temperature distributions are calculated and the shape of melting pool is determined. Furthermore, we perform microscopic thermal analysis on the nucleation and growth behaviors of ceramic hardening phases and dendrites, as well as the kinetics of related two-phase flow systems. By comparing with experimental observations, the evolution mechanisms of the morphology of Al2O3 ceramic hardening layer are explained. Based on the above results, a relationship among the scanning velocity of plasma stream, dendritic growth rate and the advancing speed of solid/liquid interface is found, and an energy criterion is proposed for predicting the pushing/engulfing transition of ceramic particles by grain growth fronts. (C) 2009 Elsevier B.V. All rights reserved.

Calorimetric study and thermal analysis of crystalline nicotinic acid

As one primary component of Vitamin B-3, nicotinic acid [pyridine 3-carboxylic acid] was synthesized, and calorimetric study and thermal analysis for this compound were performed. The low-temperature heat capacity of nicotinic acid was measured with a precise automated adiabatic calorimeter over the temperature rang from 79 to 368 K. No thermal anomaly or phase transition was observed in this temperature range. A solid-to-solid transition at T-trs = 451.4 K, a solid-to-liquid transition at T-fus = 509.1 K and a thermal decomposition at T-d = 538.8 K were found through the DSC and TG-DTG techniques. The molar enthalpies of these transitions were determined to be Delta(trs)H(m =) 0.81 kJ mol(-1), Delta(fus)H(m) 27.57 kJ mol(-1) and Delta(d)H(m) = 62.38 kJ mol(-1), respectively, by the integrals of the peak areas of the DSC curves.

CRYSTAL STRUCTURE AND THERMAL ANALYSIS OF ERBIUM COMPLEX WITH BENZENE ACETIC ACID

The crystal structure of erbium (III) complex of benzene acetic acid is reported. The complex crystallizes in the monoclinic space group P2(1)/a with a = 0,9008(3)nm, b=1.4242(5) nm, c=1.8437(7) nm, beta=98.80(3)degrees, V = 2.337(1) nm(3), Z = 4. The mechanism of thermal decomposition of complex has been studied by TG-DTG-DTA. The activation energy for dehydration reaction has been calculated by Freeman Carroll method. The enthalpy change for dehydration and phase change process has been determined.

THERMAL ANALYSIS AND INFRARED SPECTRA OF DIALKYLAMMONIUM TETRAC HLOROCUPRATE

The thermal stability and the solid solid phase transitions in Ills compounds with n = 7-12 have been studied by DSC and TG methods. Comparision with CnZn compounds want made. The nature of three phases of CnCu has been discussed in terms of infrared spectroscopy and the assignment of the phase transitions has been given. The thermal stability of CnCu is lower than that of CnZn and presents an obvious odd even effect. All of these compounds exhibit two solid solid phase transitions in the temperature range of 248-337 K. The peak tempe nature of phase transitions changes regularly. The peak temperature or the main phase transition increases with the chain length. The total transition enthalpies and entropies increase with increasing chain length. When n <= 9, the high temperature phase exists in a partial disorder state. When n >= 10, the high temperature phase exists in a conformational disorder state. The main phase transition and the phase transition at 307.7 K of CnCu may mainly are from the change of the packing structure and the change of the partial conformational order-disorder of alkyl chain, respectively.

Thermal analysis and test for single concentrator solar cells

A thermal model for concentrator solar cells based on energy conservation principles was designed. Under 400X concentration with no cooling aid, the cell temperature would get up to about 1200℃.Metal plates were used as heat sinks for cooling the system, which remarkably reduce the cell temperature. For a fixed concentration ratio, the cell temperature reduced as the heat sink area increased. In order to keep the cell at a constant temperature, the heat sink area needs to increase linearly as a function of the concentration ratio. GaInP/GaAs/Ge triple-junction solar cells were fabricated to verify the model. A cell temperature of 37℃ was measured when using a heat sink at 400X concentratration.

Thermochemical and thermal analysis on N-(p-methylphenyl)-N '-(2-pyridyl)urea

Low temperature heat capacities of N-(p-methylphenyl)-N'-(2-pyridyl)urea were determined by adiabatic calorimetry method in the temperature range from 80 to 370 K. It was found that there was not any heat anomaly in this temperature region. Based on the experimental data, some thermodynamic function results were obtained. Thermal stability and decomposition characteristics analysis of N-(p-methylphenyl)-N'-(2-pyridyl)urea were carried out by DSC and TG. The results indicated that N-(p-methylphenyl)-N'-(2-pyridyl)urea started to melt at ca. 426 K (153degreesC) and the melting peak located at 447.01 K (173.86degreesC). The melting enthalpy was 204.445 kJ mol(-1) (899.6 J g(-1)). The decomposition peak of N-(p-methylphenyl)-N'-(2-pyridyl)urea was found at 499.26 K (226.11degreesC) from DSC curve. This result was similar with that from TG and DTG experiment, in which the mass loss peak was determined as 500.4 K (227.2degreesC).

Calorimetric study and thermal analysis of berberine sulphate

The heat capacities of berberine sulphate [(C20H18NO4)(2)SO4.3H(2)O] were measured from 80 to 390 K by means of an automated adiabatic calorimeter. Smoothed heat capacities,{H-T-H-298.15} and {S-T-S-298.15} were calculated. The loss of crystalline water started at about 339.3+/-0.2 K, and its peak temperature was 365.8+/-0.6 K. The peak temperature of decomposition for berberine sulphate was at about 391.4+/-0.4 K by DSC curve. TG-DTG analysis of this material was carried out in temperature range from 310 to 970 K. TG and DSC curves show that there is no melting in the whole heating process.