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Abstract  

Differential scanning calorimetric (DSC) measurements have been carried out on Bi-Sn based amalgam precursors to be used in compact fluorescent lamps (CFLs) to study the changes in melting and solidifying behaviour caused by In dopant. The phase and elemental compositions of the samples have been characterized by using X-ray diffraction (XRD) and scanning electron microscopy-energy dispersive X-ray analysis (SEM-EDX), respectively. One of the endothermic peaks of the liquid amalgam formation shifted from 121°C to 112 and 105°C, with increasing content of 2.5 and 4.8 mass% In of samples, respectively.

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Abstract  

In this study the combustion characteristics of crude oils (Karakuę and Beykan) in the presence of a limestone matrix were determined using the thermogravimetry (TG/DTG). Experiments were performed at a heating rate of 10C min-1, whereas the air flow rate was kept constant at 10 L h-1 in the temperature range of 20-900C. In combustion with air, three distinct reaction regions were identified in all crude oil/limestone mixtures studied known as low temperature oxidation (LTO), fuel deposition (FD) and high temperature oxidation (HTO). The individual activation energies for each reaction region may be attributed to different reaction mechanisms, but they do not give any indication of the contribution of each region to the overall reactivity of the crude oils. Depending on the characteristics, the mean activation energy of samples varied between 50.3 and 55.8 kJ mol-1.

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Abstract  

Montmorillonite-supported iron(III) nitrate and copper(II) nitrate reagents, and other supported metal nitrates prepared in the same way, were investigated by thermal and X-ray powder diffraction methods. The metal nitrates are present on the support in the form of crystalline hydrate and not as acetone solvate as supposed earlier. Thermal decomposition of metal nitrates that are active in model reactions proceeds in a different way from that of the practically inactive nitrates. In the former case, water release and nitrate decomposition itself are simultaneous process. These and other results contributed to determination of suitable reaction conditions for the montmorillonite-supported reagents.

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Abstract  

A non-isothermal experimental study using thermogravimetry (TG) and differential scanning calorimetry (DSC) was conducted for investigation the oxidation reactivity of natural phosphate and its demineralised products. The analyses were carried out in oxygen atmosphere and at different heating rate (5, 10, 20, 30, 50, 60C min-1) up to 1000C. The results indicated that the material washed with HCl from the original phosphate, mainly apatite and carbonates of calcium and magnesium, as well as with HCl/HF, silicates minreals, had an inhibition effect during oxidation reactions of organic material. The increase of the heating rate shifted the reactions to higher temperatures. In addition, kinetic parameters were determined by assuming a single first-order kinetic model, using the Coats-Redfern method. The influences of demineralization process of natural phosphate and the heating rate were examined and discussed.

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Journal of Thermal Analysis and Calorimetry
Authors: E. Turi, P. Haines, V. Mathot, G. Hakvoort, T. Hatakeyama, and G. Pokol

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Abstract  

This paper discusses the changes in the structure and thermal reduction of nanosize hexagonal ammonium tungsten bronze (HATB), (NH4)0.33−xWO3−y, which were caused by K+ ion exchange (doping) and studied by XRD, XPS, 1H-MAS NMR, FTIR, SEM and TG/DTA-MS. Comparison of the cell parameters of undoped and doped HATB revealed that both a and c cell parameters decreased after the ion exchange reaction, which showed that smaller K+ ions partly replaced the larger NH4 + ions in the hexagonal channels of HATB. After the reaction, from the hexagonal channels less NH3 evolved, which also supported the incorporation of K+ ions into the hexagonal channels.

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Abstract  

A number of 30 [Co(en)3 ]Y3 , [Co(en)2 X2 ]Y and [Co(en)2 X(amine)]Y2 type complexes (X =Cl, Br; Y =Cl, Br, I, NCO, NCS, NO3 , ClO4 , etc.; amine =aromatic and alkylamines) were obtained from trans-[Co(en)2 Cl2 ]Cl by double decomposition and by substitution reactions, respectively. The structure of the complexes was proved by means of far and middle FTIR spectra. The thermal decomposition was studied by TG, DTA and DSC measurements. Mass spectra were also recorded. In the case of [Co(en)3 ]Y3 complexes the nitrate, perchlorate and dimesoperiodates decompose suddenly, frequently explosion like. The halides and thiocyanates seem to substitute an ethylenediamine ligand, yielding a rather unstable intermediate. The pyrolysis of [Co(en)2 X2 ]Y type derivatives yields no relatively stable intermediates, but the decomposition temperatures may be correlated with the nature of Y and with the cis or trans configuration of the compound. With the [Co(en)2 X(amine)]Y2 type complexes one observes the formation of [Co(en)2 XY]Y as intermediate product. From the TG curves kinetic parameters were derived for some dehydration and deamination processes, by using the nomogram method. The validity of a non-linear kinetic compensation law was observed.

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On the oximine complexes of transitionmetals

Part CXIX. Thermal and spectral studies on Ni(Diox.H)2 type chelate compounds

Journal of Thermal Analysis and Calorimetry
Authors: Cs. Várhelyi Jr., G. Pokol, Á. Gömöry, A. Gănescu, P. Sohár, G. Liptay, and Cs. Várhelyi

Abstract  

Fourteen chelates of the type [Ni(II)(Diox.H)2], ((Diox.H)2: various α-dioximes) have been studied by means of FTIR, NMR, MS data and various thermoanalytical methods (TG, DTA, DTG, DSC). In some cases kinetic parameters of the thermal decomposition of the complexes were also calculated using Zsak’s ‘nomogram method’. The mechanism of the decomposition processes was characterised on the basis of mass spectra.

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Journal of Thermal Analysis and Calorimetry
Authors: J. Bajdik, K. Pintye-Hódi, Cs. Novák, P. Szabó-Révész, G. Regdon, I. Erős, and G. Pokol

Abstract  

Dimenhydrinate is a heat-sensitive antihistamine with a low melting point. The heat-sensitive feature is of importance if direct compression is used. Direct measurement of the heat originating in the texture of tablets during compression is very difficult. Thermoanalytical methods were used as indirect methods to describe the changes in material properties at high temperature: differential scanning calorimetry, thermomicroscopy and thermogravimetric analysis. Film coating method is widely used in pharmaceutical technology. A fluidized bed apparatus was applied to coat the crystals. The coating film forming agent was hydroxy-propyl-methylcellulose (HPMC), which is a gastric-soluble polymer. Thermoanalytical measurements reveal that dimenhydrinate crystals are sensitive to heat. Film coating method does not alter the shape of the DSC curve of dimenhydrinate, but increases the melting point. The presence of a macromolecular film reduces the thermal conductivity, because it separates the particles.

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