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Thermal analysis of some fly ashes

II. Self-hardening activity of fly ashes

Journal of Thermal Analysis and Calorimetry
Authors: Z. Adonyi and K. Mészáros Szécsényi

The self-hardening activity of fly ashes was investigated looking for the possibility of their chemical reactions with water without additives. A method had to be developed for separation of the structural water from the adsorbed or free one. The decomposition of the chemically bound water was measured by thermogravimetry. The‘I’ dimensionless number proved to be applicable for the quantitative characterisation of the measured data with more DTG peaks. The examined reaction depends on the chemical composition and the physical structure of the fly ashes and the time of interaction with water. The SO3 content seems important, but the characteristics of the formed compounds differ deeply from the CaSO4·2H2O. The observed and examined reaction is an important factor of the self-hardening process of fly ash deposits.

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Abstract  

The phase diagram for the AgNO3−KNO3 system has been determined using differential scanning calorimetry (DSC). Eutectic point has been found at 391 K andX Ag=0.580 mole fraction AgNO3. The DSC curves indicate the existence of an intermermediate compound (AgNO3·KNO3) in the KNO3-rich region of the phase diagram. This compound was identified in the solid phase by X-ray diffraction. The melting and the crystallization processes were followed with the aid of a hot stage microscope, too.

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Abstract  

A method is described for the microdistillation of liquids using quasi-isothermal quasi-isobaric thermogravimetry. The liquidus curve determined under quasi-equilibrium conditions gives useful information about the composition and some thermal properties of the sample. The method could be attractive for the mineral oil, lacquer, biological and organochemical industry.

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Thermal analysis of some fly ashes

I. Gastitrimetric determination of carbon and sulfur contents of fly ashes

Journal of Thermal Analysis and Calorimetry
Authors: K. Szécsényi, M. Arnold, K. Tomor, and F. Gaál

Abstract  

The thermal behavior of different fly ashes from the electrical precipitators of various pulverized carbon fuel-fired boilers was investigated by means of simultaneous TG, DTG, DTA and EGA analysis. The carbon and sulfur contents of the samples were determined by gastitrimetry. The compositions of the samples were examined by X-ray diffraction. The quantitative oxide analysis of the ashes was carried out by means of a classical method.

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Abstract  

Manganese(II) chloride complexes with 3,4- and 3,5-lutidine have been prepared. The crystal symmetry and cell dimensions have been calculated on the basis of powder diffraction data. The compounds were characterised also by FT-IR spectrometry. The thermal decomposition of the complexes has been studied by thermogravimetry and DSC. By plotting densities vs. molar mass, the diagram obtained has correspondence to similar observations in other solid metal-lutidine complex systems.

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Transition metal complexes with thiosemicarbazide-based ligands

31. Dioxouranium(VI) complexes with N(1),N(4)-bis(salicyIidene)- and N(1)-benzoylisopropylidene-N(4)-saIicylidene-S-alkyl-isothio-semicarbazides

Journal of Thermal Analysis and Calorimetry
Authors: V. Leovac, E. Ivegeš, K. Szécsényi, K. Tomor, G. Pokol, and S. Gal

Abstract  

Solvate complexes of UO2 2+ andN(1), N(4)-bis(salicylidene)-S-methylisothiosemicarbazone, (H2Me-L1), of general formula [UO2(Me-L1)S] (S= H2O, MeOH, EtOH, Py, DMF and DMSO) were synthesized. The methanolic UO2 2+” adducts of N(1)-benzoylisopropylidene-N(4)-salicylidene-S-alkylisothiosemicarbazone, (H2R-L2,R=Me, Prn) of general formula [UO2(R-L2)· MeOH], were also prepared. Thermal decomposition of the complexes was investigated in air and argon. The complexes decompose to α-U3O8 in air, while in argon the decomposition is not completed up to 1000 K. The temperature and the mechanism of decomposition of the complexes are a function of the solvent belonging to the inner coordination sphere.

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Abstract  

Triammonium-N-dithiocarboxyiminodiacetate, (NH4)3L, a new dithiocarbamato derivative of iminodiacetate, has been synthesized. The coordination properties of the ligand were tested in reactions with copper(II), nickel(II) and palladium(II) salts in acidic solutions. Complexes with a general formula M(H2L)2 were obtained, with the coordination taking place through the sulfur atoms of the dithiocarbamate moiety. The new compounds were characterized by elemental analysis, UV/VIS and IR spectroscopy, thermal analysis and magnetic measurements. In addition, the ligand was characterized by 1H- and 13C-NMR spectroscopy and molar conductivity measurements. The copper(II) complex is paramagnetic, while the nickel(II) and palladium(II) compounds are diamagnetic. The thermal decomposition of all compounds is continuous and the thermal stability of the complexes is higher than that of the ligand, as expected.

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Abstract  

Compounds obtained by a solid–gas phase reactions between copper(II) chloride and bromide and 2,4-, 2,6- 3,4- and 3,5-lutidines were studied using thermogravimetry, far-infrared, electronic spectroscopy and X-ray diffraction. The results were compared with the corresponding data for the similar compounds with methylpyridines and 2,4,6-collidine. A special attention was paid to the host-guest phenomenon, a new structural feature of transition-metal halide complexes.

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Abstract  

We report the synthesis and the characterization (elemental analysis, FT-IR spectroscopy, thermal methods and molar conductivity measurements) of the mixed complexes of zinc with acetate and 3-amino-5-methylpyrazole, HL 1, [Zn(OAc)2(HL1)2], or 3-amino-5-phenylpyrazole, HL 2 [Zn(OAc)2(HL2)2], or 4-acetyl-3-amino-5-methylpyrazole, HL 3, [Zn(OAc)(L3)(HL3)]2, with isothiocyanate and HL 2 [Zn(SCN)2(HL2)2], or HL 3 [Zn(SCN)2(HL3)2], and with nitrate, isothiocyanate and 3,5-dimethyl-1-carboxamidinepyrazole, HL 4 [Zn(NO3)(NCS)(HL4)2]. The thermal decomposition of the complexes is generally continuous resulting zinc oxide as end product,except [Zn(OAc)(L3)(HL3)]2 in which case a well-defined intermediate was observed between 570–620 K. On the basis of the IR spectra and elemental analysis data of the intermediate a decomposition scheme is proposed.

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