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.5–6%, also depending on the climatic regions in Europe ( Rademacher and Harz, 2006 ), above which the mortality rates increase in bees. In Hungary, which has one of the highest bee densities in Europe, sublimation of OA is considered to be one of the most

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Abstract  

Procedures for measuring sublimation rates of pharmaceutical compounds by isothermal thermogravimetry are discussed. Experimental data was obtained using the Mettler TA4000 thermogravimetric system. The sublimation rate is measured directly from the mean weight loss per unit time in the linear region of the monitored TG profile at a set isothermal temperature. This data when fitted to the Arrhenius equation yields the sublimation enthalpy. For the benzoic acid reference, the enthalpy so calculated is 99% of the value obtained from direct vacuum TG measurements. Thermal degradation in the solid state or pre-melting can effect a departure from the characteristic linear mass loss-time sublimative profile. Data pertaining to several established Merck drugs is discussed. Examples where loss of residual solvent, onset of thermal degradation and pre-melting phenomena affect the measurement, are presented.

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5-Nitro-8-hydroxyquinoline (B) and 5,7-dinitro-8-hydroxyquinoline (C) were obtained from nitration of 8-hydroxyquinoline (A) and purified in acetone medium and under heating in which the formation of (B) or (C) depends on the amount of HNO3 added. TG curves present mass loss in only one step before and after the melting point (T m =76C (A) and 180C (B)) in different proportions as a function of the heating rate, characterising the sublimation and the volatilisation processes, respectively. The thermal stability of the compounds follow the order: A (77C)<B (121C)<C (222C). Kinetic parameters through TG curves, dynamic process, using heating rates of 1, 2.5, 5, 10 and 20C minȡ1 , enabled to obtain the following increasing order to the activation energy values of the compounds: 80.4 (A), 102.0 (B) and 153.9 kJ mol−1 (C). Other kinetic parameters as pre-exponential and half-lifetime were also estimated.

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Investigation on the nature of an initial mass loss observed for Mn(II)pyrrolidinedithiocarbamate complex is described. No evidences of decomposition are observed in infrared or mass spectra, elemental analysis and scanning electron microscopy of the residue at the end of the first thermal event, when compared with the same data for the original complex. Partial sublimation is assigned as the physical event after several experiments. The results are comparable with the findings for other complexes of the first transition series with pirrolidinedithiocarbamate.

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TNAZ (1,3,3-trinitroazetidine) is a relatively new, powerful, steam castable, strained ring explosive. Owing these characteristics it is of considerable interest to the energetic material community. A relatively high vapour pressure, volume contraction and formation of shrinkage cavities in the solidification of its melt may be considered as some of its disadvantages. The kinetics and heats of TNAZ sublimation and evaporation were studied by the non-isothermal and isothermal thermogravimetry method. The activation energy of 94-102 kJ mol-1 was found for TNAZ sublimation, while the activation energy of 60-81 kJ mol-1 was found for TNAZ evaporation. The enthalpy of TNAZ sublimation at the melting temperature was found to be 95 kJ mol-1, and the enthalpy of TNAZ evaporation equals 66 kJ mol-1.

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Temperature dependences of solubility, saturated vapour pressure and crystal heat capacity of [4-(Benzyloxy)phenyl]acetic acid were determined. The solubility of this compound was investigated in n-hexane, buffered water solutions with pH 2.0 and 7.4 and n-octanol. The enthalpy of sublimation and vaporization as well as the fusion temperature were determined. Solvation and solubility processes have been analyzed. The thermodynamics of transfer processes from one buffer to another (protonation process), from buffers to 1-octanol (partitioning process), and from n-hexane to the applied solvents (specific interaction) have been calculated and compared to those of other NSAIDs. The relevant shares of specific and non-specific interactions in the process of solvation have been investigated and discussed.

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Introduction Correlations between the enthalpy of sublimation and the temperature of sublimation at a reference pressure, or between the enthalpy of sublimation and the standard Gibbs energy of sublimation at 298.15 K have been

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. Thermogravimetry analysis (TG) is the most widely used technique in measuring sublimation rates of different materials. TG often requires a flow of gas through both the balance chamber and the sample to prevent temperature and pressure build-up [ 1 – 3 ]. However

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The volatile scandium-β-diketonates are synthesised using acetylacetone (acac) and tetramethylheptanedione (tmhd) as coordinative ligands for CVD application. The X-ray powder patterns are indexed and analysed and found to be orthorhombic and monoclinic phases for Sc(acac)3(1) and Sc(tmhd)3(2) respectively. The sublimation and evaporation kinetics have been analyzed using three calculating techniques. The non-isothermal based activation energy values are found to be 38 ± 2 and 73 ± 2 kJ mol−1 by Flynn–Wall technique for (1) and (2) respectively. The measured Ea values are close to the value obtained using Kissinger method.

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The standard (p 0=0.1 MPa) molar enthalpy of formation, Δf H 0 m, for crystalline N-phenylphthalimide was derived from its standard molar enthalpy of combustion, in oxygen, at the temperature 298.15 K, measured by static bomb-combustion calorimetry, as –206.03.4 kJ mol–1. The standard molar enthalpy of sublimation, Δg cr H 0 m , at T=298.15 K, was derived, from high temperature Calvet microcalorimetry, as 121.31.0 kJ mol–1. The derived standard molar enthalpy of formation, in the gaseous state, is analysed in terms of enthalpic increments and interpreted in terms of molecular structure.

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