GaPO4 high temperature crystal microbalance demonstration up to 720°C

Quartz-homeotypic gallium (ortho-) phosphate, GaPO₄, is of special interest for resonator applications asking for temperature compensated cuts with higher electro-mechanical coupling than quartz and operational temperatures up to 970°C. The crystal microbalance technique, well known for quartz (QCM) which can be used only at moderate temperatures, can now be extended to much higher temperatures using GaPO₄ crystals, benefiting from all three advantages mentioned above. Two different experiments were done to demonstrate the advantages of a crystal microbalance based on GaPO₄. First, the GaPO₄ resonator was used for film thickness determination and compared with a commercial QCM. This experiment demonstrated that the measuring range can be extended by using GaPO₄ resonators instead of quartz. The second experiment demonstrates the possibility for thermogravimetric analysis up to 720°C by using a new concept for resonator mounting.This revised version was published online in November 2005 with corrections to the Cover Date.     

铁催化剂在碳—氧反应中的热重研究

采用动态TG－DTG，研究了铁催化剂的制备方法、前驱化合物的 种类及 热处理对其在碳－氧反应中催化活性的影响。观察到在干混法制备催化剂时，所用铁盐分解温度越低活性越高。此外还发现，热处理可明显提高由分解温度高的含氧铁盐制备的 催化剂的活性，但对于不含氧铁盐和分解温度低的含氧铁盐无影响。     

Thermogravimetric study of polyacrylamide with evolved gas analysis

Dried samples of polyacrylamide in an He atmosphere have been subjected to thermogravimetric analysis in the 30–600°C range, and the evolved gases were monitored by FTIR. Water, ammonia, and small quantities of carbon dioxide are released in the first stages of decomposition (220–340°C), where the polymer chains remain intact and the reaction occurs on the pendant amide groups. In the second stage of decomposition (340–440°C), the majority of the weight loss occurs, and main chain breakdown occurs, releasing carbon dioxide, water, nitrile compounds, and imides. Trapping of the gases in this stage and analysis by GC–FTIR and GC–MS reveals the presence of more than 20 decomposition products, and confirms that a large proportion of these can be assigned to glutarimide and its substituted analogs. Imidization and dehydration reactions on the amide groups, as well as free radical breakdown of the main chains, with inter- and intramolecular hydrogen transfer, can account for many of the products of the decomposition. © 1993 John Wiley & Sons, Inc.     

Using ordinary differential equations system to solve isoconversional problems in non-isothermal kinetic analysis

The mathematical evaluation of the activation energy, E, of non-isothermal degradation reactions is usually made using the Ozawa/Flynn–Wall isoconversion principle and involves the numerical resolution of a set of integrals without closed form solution, which are solved by polynomial approximation or by numeric integration. In the present work, the isoconversion principle, originally described and maintained until now as an algebraic problem, was written as a set of ordinary differential equations (ODEs). The individual ODEs obtained are integrated by numeric methods and are used to estimate the activation energy of simulated examples. A least square error (LSE) objective function using the introduced ODEs was written to deal with multiple heating rate CaCO₃ thermal decomposition TG experiments.     

Thermal behaviour and slow molecular mobility in two isomers of biphenylmethanol

This research was aimed to investigate the role of clay on the combustion and kinetic behavior of crude oils in limestone matrix. For this purpose, simultaneous TG (thermogravimetry) and DTA (differential thermal analysis) experiments were performed at three different heating rates as 10–15 and 20°C min^–1, respectively. A uniform trend of decreasing activation energies was observed with the addition of clay. It was concluded that clays surface area affects the values of Arrhenius constant, while it is the catalytic properties of clay, which lower the activation energies of all the reactions, involved in the combustion process.     

Effect of the complex forming ion on the physicochemical characteristics of solvation of tetraphenylporphine complexes

The enthalpies of dissolution, transfer, and axial coordination for the Cd(II), Co(II), Mn(III), Fe(III), and Cr(III) complexes of tetraphenylporphine, H₂(TPP), in nonpolar (C₆H₆, CCl₄) and electron-donating solvents (DMF, DMSO, Py,c-C₅H₁₀NH) have been determined calorimetrically at 298.15 K. On the basis of thermogravimetrical data for the corresponding crystallosolvates the composition, thermal stability, and energy of intermolecular interaction of the metal-porphine complexes with pyridine have been calculated. Complexing in noncoordinating solvents brings about no radical change in the physicochemical characteristics of axial coordination which depend critically on the electron structure of the complex-forming metal.Translated fromfzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 846–850, May, 1993.     

Thermal degradation of vinylidene chloride/vinyl chloride copolymers in the presence of N-substituted maleimides

As a consequence of their excellent barrier properties vinyl chloride/vinylidene chloride copolymers have long been prominent in the flexible packaging market. While these polymers possess a number of superior characteristics, they tend to undergo thermally- induced degradative dehydrochlorination at process temperatures. This degradation must be controlled to permit processing of the polymers. Three series of N-substituted maleimides (N-alkyl-, N-aralkyl, and N-aryl) have been synthesized, characterized spectroscopically, and evaluated as potential stabilizers for a standard vinyl chloride/vinylidene chloride (85 mass%) copolymer. As surface blends with the polymer, these compounds are ineffective as stabilizers. However, significant stabilization may be achieved by pretreatment of the polymer with N-substituted maleimides. The most effective stabilization of the polymer is afforded by N-aralkyl- or N-arylmaleimides, most notably, N-benzylmaleimide and N-p-methoxyphenylmaleimide.     

Thermogravimetric properties of inclusion complexes ofβ-cyclodextrin with benzene,acetylsalicylic acid and methyl salicylate

This paper reports TG analyses of inclusion complexes of-cyclodextrin with benzene, acetylsalicylic acid and methyl salicylate. The data were used for calculation of the compositions of the three body complexes and the apparent kinetic parameters of the thermal decompositions. Water exclusion proceeds as a reaction with ordern=1 and an activation energy about 20 kJ/mol. The expulsion of aromatic guest molecules follows ann=1 order process with the activation energy above 155 kJ/mol, except that for the methyl salicylate complex, which was found to be ca. 64 kJ/mol.     

The investigation of ancient pottery

Summary Ancient ceramic samples (single fragments and different parts of pots, unbroken and repaired; total about 180 samples) dated from the transitional period of late Bronze to early Iron Age (VIII-VI centuries BC) and early Iron Age (VII-IV centuries BC) were investigated by thermal analysis, X-ray powder diffraction, petrography, and scanning electron microscopy equipped with the energy-dispersive X-ray analyzer. In addition to that, to identify the clay sources for the ceramic manufacturing, about 15 samples of clays and soils found near archeological digs and taken from the mineralogical museum were investigated. We found out that the calcite content of ceramics is a very informative parameter for the identification of the clay source for the pottery manufactured at low technological level (low-temperature firing).     

Thermal Stability of a Para-Cresol Novolac Resin

The thermal stability of p-cresol novolac resin was studied by means of DSC, X-ray diffraction, thermogravimetry and SEC investigations. After 30 thermal cycles in which the same sample was heated, cooled and heated again, without attainment of the temperature of degradation at any time in the experiment, important structural modifications are observed. At the end of the experiments, the resin, which is initially highly crystalline, exhibits all the characteristics of a semi-crystalline material. This revised version was published online in July 2006 with corrections to the Cover Date.