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B2636 - Energetics of coumarin and chromone
Condensed phase standard (p degrees = 0.1 MPa) molar enthalpies of formation for coumarin and chromone were derived from the standard molar enthalpies of combustion, in oxygen, at T = 298.15 K, measured by static bomb combustion calorimetry. The standard molar enthalpies of sublimation, at T = 298.15 K, were measured by Calvet microcalorimetry. Combining these values, the following enthalpies of formation in the gas phase, at T = 298.15 K, were then derived: coumarin, -(163.4 3.3) kJ x mol(-1), and chromone, -(126.1 2.5) kJ x mol(-1). The temperatures of fusion, T(fusion), and fusion enthalpies, at T = T(fusion), were also reported. Additionally, theoretical calculations were done using different methods: DFT/B3LYP, MCCM (MC-UT/3 and MC-QCISD/3), and also the more accurate G3MP2 method. Good agreement between experimental and theoretical data was achieved. Some correlations between structure and energy were also made, and the aromaticity of the compounds was evaluated by the nucleus independent chemical shifts (NICS).
M Agostinha R Matos, Clara C S Sousa, Margarida S Miranda, Victor M F Morais, Joel F Liebman , The Journal of Physical Chemistry B (2009) 113, 11216-11221
B2635 - Recording of continuous cooling precipitation diagrams of aluminium alloys
The purpose of this report is to present a methodology to record continuous cooling precipitation (CCP) diagrams over the complete range of technical interesting cooling rates for some aluminium wrought alloys. With the information out of CCP-diagrams, the quenching step of the heat-treatment process ÒAge HardeningÓ can be optimized. The nanosized precipitations were detected via Differential Scanning Calorimetry (DSC) by identifying their exothermal heat. Aluminium wrought alloy EN AW-6005A was age hardened in three different DSCs whereby cooling rate range varies over 3 orders of magnitude. With increasing cooling rate, the precipitation heat is decreasing. The CCP-diagram covers cooling rates form close to equilibrium conditions at 0.1 K/min up to the critical cooling rate at 375 K/min where the precipitation reaction is suppressed completely. The DSC delivers a very useful method to record full range CCP-diagrams of aluminium alloys. Opposite to other possible methods, it also delivers a measure for the amount of the nanosized precipitates by the amount of released heat. A strategy is presented for the deconvolution of overlapping DSC-peaks.
Benjamin Milkereit, Olaf Kessler, Christoph Schick, Thermochimica Acta, 492 (2009) 73Ð78
B2634 - Precipitation kinetics of an aluminium alloy during Newtonian cooling simulated in a differential scanning calorimeter
The purpose of this report is to compare linear and non-linear cooling with respect to the precipitation behaviour of aluminium alloy EN AW-6082. Therefore an approximation of gas cooling by Newtonian law was performed. However, DSCs are typically designed for linear scanning. Hence a completely new method has been developed, to perform DSC-experiments during non-linear cooling. The temperature/time profile for two different types of DSCs was optimized avoiding overshoots at each change of cooling rate. Smooth curves were obtained by normalizing the measured heat flow rate by the actual heating rate yielding excess heat capacity as function of temperature. For the investigated aluminium alloy EN AW-6082 both kinds of cooling, linear and Newtonian, delivered comparable information about the characteristic precipitation reactions. Essential parts of the continuous cooling precipitation diagram could be recorded for both types of cooling. The intensities of the reactions, measured by the specific precipitation heat, were similar.
Benjamin Milkereit, Martin Beck, Michael Reich, Olaf Kessler, Christoph Schick, Thermochimica Acta, 522 (2011) 86Ð95
B2633 - Shape-dependent surface energetics of nanocrystalline TiO2
We report the direct determination of surface enthalpies for nanophase TiO2 anatase with different morphologies derived from drop solution calorimetry in a molten sodium molybdate (3Na2O?4MoO3) solvent at 702 ¡C. The energetics of surface hydration has been measured using a Calvet microcalorimeter coupled with a gas dosing system. The surface enthalpies of hydrated surfaces for anatase TiO2 nanoparticles, nanowires and sea-urchin-like assemblies are 0.51 ± 0.05, 1.07 ± 0.28, and 1.29 ± 0.16 J m?2, respectively, whereas those of anhydrous surfaces are 0.74 ± 0.04, 1.24 ± 0.28, and 1.41 ± 0.16 J m?2, respectively. The trend in TiO2, which shows higher surface enthalpies for more complex nanostructures, is consistent with that reported in ZnO. The shape-dependent surface enthalpy at the nanoscale level is discussed in terms of exposed surface structures. The enthalpies of hydration appear to be similar for all morphologies
Tae-Jin Park , Andrey A. Levchenko , Hongjun Zhou , Stanislaus S. Wong, Alexandra Navrotsky, J. Mater. Chem., 2010, 20, 8639-8645
B2632 - Thermal analyses to assess diffusion kinetics in the nano-sized interspaces between the growing crystals of a glass ceramics
According to a hypothesis by Rssel and coworkers, the absence of Ostwald ripening during isothermal crystallization of lithium aluminosilicate (LAS) and other glass ceramics indicates the existence of a kinetic hindrance of atomic reorganization in the interstitial spaces between the crystals. Methods of Thermal Analysis (Differential Scanning Calorimetry (DSC), Dynamic Mechanical Analysis (DMA)) which are sensitive to the local atomic rearrangements in the interstitial spaces (including viscous flow) are applied to find support for the idea of kinetic hindrance and the formation of a core shell structure acting as diffusion barrier. Both the DSC-measured calorimetric glass transition and the DMA-measured viscoelastic properties indicate an increase in the time constants of atomic rearrangements and diffusion by at least two orders of magnitude during ceramization. This fits to the above idea. Based on these findings, thermo analytic studies have been performed in order to find out how Ostwald ripening may be provoked.
Ulrich Fotheringham, Roman Wurth, Christian Rssel, Thermochimica Acta, 522 (2011) 144Ð150
B2631 - Refined heat capacity of LaPO4 in the temperature range 0Ð1600 K
The critical analysis of literature heat capacity data in the temperature range 0Ð1600 K was carried out. It was shown that joining of Cp(T) curves obtained by the different methods was performed improperly. Experimental heat capacity of LaPO4 was measured in the region 16Ð324 K by the adiabatic calorimetry. The obtained data allows to consist the results of different works and to fit the lanthanum orthophosphate heat capacity in the wide temperature range. Standard thermodynamic properties were calculated on the basis of the refined heat capacity data: = 102.5 ± 0.2 J K?1 mol?1, S0(298.15 K) = 108.7 ± 0.2 J K?1 mol?1, H0(298.15 K) ? H0(0 K) = 17.44 ± 0.03 kJ mol?1, ?0(298.15 K) = 50.21 ± 0.20 J K?1 mol?1.
K.S. Gavrichev, M.A. Ryumin, A.V. Tyurin, V.M. Gurevich, L.N. Komissarova, Thermochimica Acta, 474 (2008) 47Ð51
B2630 - Heat capacities of several AlÐNiÐTi compounds
The heat capacities of several AlÐNiÐTi compounds were determined by drop calorimetry over the temperature range of 500Ð1500 K. A modified Einstein model and a two-parameter polynomial model provide reasonable representations of the experimental heat capacity data. The heat capacities, Cp, using a two-parameter polynomial representation are as follows: Ni0.5Ti0.5, Cp = 22.39 + 8.24 ? 10?3 T (J/(mol K)); Al0.45Ni0.5Ti0.05, Cp = 23.01 + 5.12 ? 10?3 T (J/(mol K)); Al0.16Ni0.74Ti0.10, Cp = 18.36 + 10.76 ? 10?3 T (J/(mol K)); and Al0.25Ni0.5Ti0.25, Cp = 25.38 + 1.088 ? 10?3 T (J/(mol K)). The experimental data are compared with the values derived from a thermodynamic database of Gibbs energy functions. The analysis shows that (1) either model is a good representation of the data; (2) it is not adequate to assume the Neumann-Kopp rule for the description of the heat capacities of Al0.45Ni0.5Ti0.05, Al0.16Ni0.74Ti0.10 and Al0.25Ni0.5Ti0.25; (3) it is not appropriate to determine a compound Cp from a thermodynamic database of Gibbs energy functions if the compound is modeled by using the Neumann-Kopp rule and any of its components undergoes melting in the temperature range of interest.
Rongxiang Hu, Philip Nash, Qing Chen, Lijun Zhang, Yong Du, Thermochimica Acta, 486 (2009) 57Ð65
B2629 - Calorimetric measurements on plutonium rich (U,Pu)O2 solid solutions
Enthalpy increments of U(1?y)PuyO2 solid solutions with y = 0.45, 0.55 and 0.65 were measured using a high-temperature differential calorimeter by employing the method of inverse drop calorimetry in the temperature range 956Ð1803 K. From the fit equations for the enthalpy increments, other thermodynamic functions such as heat capacity, entropy and Gibbs energy function have been computed in the temperature range 298Ð1800 K. The results are presented and compared with the data available in the literature. The results indicate that the enthalpies of U(1?y)PuyO2 solid solutions with y = 0.45, 0.55 and 0.65 obey the NeumannÐKopp's molar additivity rule.
R. Kandan, R. Babu, K. Nagarajan, P.R. Vasudeva Rao, Thermochimica Acta, 472 (2008) 46-49
B2628 - Thermodynamic functions of Ba10(PO4)6Cl2, Sr10(PO4)6Cl2 and Ca10(PO4)6Cl2
Alkaline earth chloroapatites, M10(PO4)6Cl2 (M = Ba, Sr, Ca) were prepared by solid state reaction route and characterized by XRD. The lattice constants of Ba10(PO4)6Cl2, Sr10(PO4)6Cl2, Ca10(PO4)6Cl2 were determined to be a = 10.27(1) , c = 7.66(1) ; a = 9.87(2) , c = 7.18(1) and a = 9.52(1) , c = 6.85(1) respectively. The enthalpy increments were measured by inverse drop calorimetric method in the temperature range 523Ð1423 K using a high temperature calorimeter. Thermodynamic functions such as heat capacity, entropy and Gibbs energy functions in the temperature range 298Ð1500 K, were computed from the measured enthalpy increments.
R. Babu, Hrudananda Jena, K.V. Govindan Kutty, K. Nagarajan, Thermochimica Acta, 526 (2011) 78Ð82
B2627 - Thermochemistry of PdÐIn, PdÐSn and PdÐZn alloy systems
The standard enthalpy of formation of several PdÐM alloys (M = In, Sn and Zn) has been measured using a high temperature direct drop calorimeter. The reliability of the calorimetric results has been determined and supported by using different analytical techniques: light optical microscopy, scanning electron microscopy equipped with electron probe microanalysis (EPMA with EDS detector) and X-ray powder diffraction analysis. The values of ?fH (kJ/mol atoms) for the following phases were obtained for the formation in the solid state at 300 K: PdIn (49 at.%In): ?69.0 ± 1.0; Pd2In3 ?57.0 ± 1.0; Pd3In7: ?43.0 ± 1.0; PdSn2: ?50.0 ± 1.0; Pd2Zn9 (77 at.%Zn): ?33.7 ± 1.0; Pd2Zn9 (78 at.%Zn): ?34.0 ± 1.0; Pd2Zn9 (80 at.%Zn): ?35.0 ± 1.0. The results show exothermic values which increase from the PdÐZn to the PdÐSn and PdÐIn systems; the data obtained have been discussed in comparison with those available in literature
S. Amore, S. Delsante, N. Parodi, G. Borzone, Thermochimica Acta, 481 (2009) 1-6
B2626 - Partial and integral enthalpies of mixing of AgÐGaÐSn liquid alloys
A Calvet type calorimeter was used for measurement of partial and integral enthalpies of mixing of AgÐGaÐSn alloys. The AgÐGa binary alloys have been studied with 0 < xAg < 0.79 composition and in the 803Ð1073 K temperature range. The mixing enthalpies at 803 K of GaÐSn binary alloys have been determined for xSn < 0.35. The AgÐGaÐSn ternary liquid alloys have been investigated at 803 K along the following sections: xAg/xGa = 1/3, xAg/xGa = 0.36/0.64, xAg/xGa = 1/1, xGa/xSn = 1/3, xGa/xSn = 1/1, xGa/xSn = 0.65/0.35 and xGa/xSn = 3/1. Experimental data were used to obtain the binary interaction parameters by using the RedlichÐKister polynomial for the AgÐGa binary system, while the RedlichÐKisterÐMuggianu method was used to determine the ternary interaction parameters for the AgÐGaÐSn system. The experimental values and the fitted curves were compared with those predicted from the Muggianu and Toop methods.
D. Li, S. Delsante, W.Gong, G. Borzone, Thermochimica Acta, 523 (2011) 51-62
B2625 - Heat contents of the intermetallics V3Ge and V5Ge3 and thermodynamic modeling of the GeÐV system
Fourteen alloys were prepared by arc-melting the pure elements and annealing the alloys at 850 ¡C for 30 days. The annealed alloys were examined by XÐray diffraction (XRD), scanning electron microscope with energy dispersive X-ray analysis (SEM/EDX), differential scanning calorimetry (DSC) and drop calorimeter. The major experimental results are as follows. (I) The heat contents of V3Ge and V5Ge3 were measured by drop calorimeter from 400 to 900 ¡C. (II) The microstructure analysis of as-cast alloy V87.1Ge12.9 indicates that the eutectic composition of liquid ? (V) + V3Ge is above 12.9 at.% Ge, and that of V2.9Ge97.1 shows that the eutectic composition of liquid ? V17Ge31 + Ge is close to 97.1 at.% Ge. (III) The invariant reaction temperatures of liquid + V11Ge8 ? V17Ge31 and liquid ? V17Ge31 + Ge are at 960.0 ± 2 ¡C and 930.7 ± 2 ¡C, respectively. Based on the experimental results in this study and in the literature, the GeÐV system was modeled by CALPHAD approach.
Xiaoming Yuan, Weihua Sun, Yoonsung Chung, Honghui Xu, Shuhong Liu, Yong Du, Philip Nash, Dewen Zeng, Thermochimica Acta, 513 (2011) 100Ð105
B2624 - Enthalpies of mixing of liquid systems for lead free soldering: AlÐCuÐSn system
The present work refers to high-temperature drop calorimetric measurements on liquid AlÐCu, AlÐSn, and AlÐCuÐSn alloys. The binary systems have been investigated at 973 K, up to 40 at.% Cu in case of AlÐCu, and over the entire concentrational range in case of AlÐSn. Measurements in the ternary AlÐCuÐSn system were performed along the following cross-sections: xAl/xCu = 1:1, xAl/xSn = 1:1, xCu/xSn = 7:3, xCu/xSn = 1:1, and xCu/xSn = 3:7 at 1273 K. Experimental data were used to find ternary interaction parameters by applying the RedlichÐKisterÐMuggianu model for substitutional solutions, and a full set of parameters describing the concentration dependence of the enthalpy of mixing was derived. From these, the isoenthalpy curves were constructed for 1273 K. The ternary system shows an exothermic enthalpy minimum of approx. Ø18,000 J/mol in the AlÐCu binary and a maximum of approx. 4000 J/mol in the AlÐSn binary system. The AlÐCuÐSn system is characterized by considerable repulsive ternary interactions as shown by the positive ternary interaction parameters.
Hans Flandorfer, Meryem Rechchach, A. Elmahfoudi, Lszl-- Bencze, Arkadij Popovic, Herbert Ipser, J. Chem. Thermodynamics 43 (2011) 1612Ð1622
B2623 - The role of aromatic interactions in the structure and energetics of benzyl ketones
A qualitative and quantitative energetic and structural study of dibenzyl ketone (DBK) and benzyl ethyl ketone (BEK) was carried out in order to obtain insights into the type and magnitude of aromatic interactions that these systems present in their different phases. The crystal structure of DBK was obtained by X-ray crystallography, and it shows that the conformation adopted in the crystalline state is governed by the intermolecular interactions. The standard (p0 = 105 Pa) molar enthalpy of formation in the gaseous state at T = 298.15 K was derived by Calvet and combustion calorimetry. Using a homodesmic reaction scheme, the first calorimetric evaluation of the interaction enthalpy between two stacked phenyl rings is presented. A stabilizing enthalpic effect of (12.9 ± 4.9) kJ mol?1 associated with the intramolecular ¹Ð¹ interaction in DBK was found. The gas phase intramolecular ¹¹ interaction in DBK is in agreement with quantum chemical calculations at B3LYP/6-311++G(d,p) and MP2 with various basis-sets. An intramolecular ¹¹ interaction in DBK and a weak CÐH¹ interaction in BEK were found by variable-temperature 1H-NMR spectroscopy in MeOD. These observations are consistent with a hindered rotor interpretation, supported by ab initio calculations for the gas phase at the MP2/cc-pVDZ level. The global results indicate a distinct molecular structure on going from crystalline DBK to liquid, gas, and solution phases, ruled by the overall contribution of the intra- and intermolecular interactions.
Carlos F. R. A. C. Lima , Carlos A. D. Sousa , Jos E. Rodriguez-Borges , Andr Melo , L'gia R. Gomes , John N. Low and Lu's M. N. B. F. Santos, Phys. Chem. Chem. Phys., 2010, 12, 11228-11237
B2622 - Calorimetric and computational study of 7-hydroxycoumarin
The standard (p¡ = 0.1 MPa) molar energy of combustion in oxygen, at T = 298.15 K, of 7-hydroxycoumarin was measured by static bomb calorimetry. The value of the standard molar enthalpy of sublimation was obtained by Calvet microcalorimetry and corrected to T = 298.15 K. Combining these results, the standard molar enthalpy of formation of the compound, in the gas phase, at T = 298.15 K, has been calculated, ?(337.5 ± 2.3) kJ á mol?1. The values for the temperature of fusion, Tfusion, and for the fusion enthalpy, at T = Tfusion, are also reported. Additionally, high-level density functional theory calculations using the B3LYP hybrid exchange-correlation energy functional with extended basis sets, the MC3BB and MC3MPW methodsand more accurate correlated computational techniques of the MCCM suite have been performed for the compound. The agreement between experiment and theory gives confidence to estimate the enthalpy of formation of the remaining hydroxycoumarins substituted in the benzene ring.
Clara C.S. Sousa, M. Agostinha R. Matos, Victor M.F. Morais, The Journal of Chemical Thermodynamics, 43 (2011) 1435Ð1440
B2621 - Calorimetric Investigation of PrBr3-MBr Liquid Mixtures (M = Na, K, Rb, Cs)
The molar enthalpies of mixing (?mixHm) in liquid alkali bromide-praseodymium(III) bromide mixtures have been measured with a Calvet-type high temperature microcalorimeter over the entire composition range at 1070 K. All of the melts are characterized by negative enthalpies of mixing with a minimum value shifted toward the alkali bromide-rich compositions that are located in the vicinity of x(PrBr3)?0.4. The magnitude of the mixing enthalpy depends on the ionic radius of the alkali metal, radius of the common halide ion, and the ionic radius of the lanthanide(III) cation.
Leszek Rycerz, Marcelle Gaune-Escard, J. Chem. Eng. Data, 2011, 56, 3273Ð3276
B2620 - Calorimetric Investigation of the CeBr3-MBr Liquid Mixtures (M = Na, K, Rb, Cs)
The molar enthalpies of mixing (?mixHm) in the liquid cerium(III)?alkali metal bromide mixtures were measured with a Calvet- type high temperature microcalorimeter over the entire composition range at 1073 K. Mixing the two liquid components was achieved by using the Òbreak-off ampule techniqueÓ. All the melts are characterized by negative enthalpies of mixing with a minimum value of approximately ?5.3 kJámol?1, ?12.7 kJámol?1, ?16.1 kJámol?1, and ?18.4 kJámol?1, for M = Na, K, Rb, and Cs, respectively. For all the systems, the minimum of the enthalpy of mixing is shifted toward the alkali bromide-rich compositions and located in the vicinity of x(CeBr3) 0.4. The composition dependence of the interaction parameter ?, with a broad minimum at x(CeBr3) 0.2 for the systems with KBr, RbBr, and CsBr is indicative of LnBr63? complexes formation in the melts.
Leszek Rycerz, Marcelle Gaune-Escard, J. Chem. Eng. Data, 2009, 54, 2622Ð2625
B2619 - Enthalpy of formation of the LaÐMg intermediate phases
The aim of this work is to complete the available set of thermodynamic data on the LaÐMg system in order to get reliable optimisation of this system by the CALPHAD method. Indeed the CALPHAD method requires a large set of consistent input data including both phase diagram and thermodynamic data. The enthalpies of formation of the LaÐMg intermediate compounds were determined at 298 K by means of solution calorimetry in liquid Sn in a TianÐCalvet calorimeter. In these experiments, the partial enthalpies of solution of the compounds at infinite dilution in liquid tin were measured at 665 K. The enthalpies of formation of LaMg, LaMg2 and La2Mg17 compounds were also calculated at 0 K by density functional theory to compare experimental and calculated values.
A. Berche, F. Marinelli, J. Rogez, M.-C. Record, Thermochimica Acta, 499 (2010) 65Ð70
B2618 - Calorimetric investigations of AuÐIn, InÐSb and AuÐInÐSb systems at 973 K
The molar enthalpies of mixing of the AuÐIn, InÐSb and AuÐInÐSb alloys have been determined at 973 K using a Calvet hightemperature microcalorimeter by the drop method. Measurements in the ternary system AuÐInÐSb were performed along four sections, xAu/xIn = 1/3Ð1/1 and xIn/xSb = 1/1Ð3/1. The experimental calorimetric data and estimated values with a RedlichÐKisterÐMuggianu formulation are compared.
S. Hassam, D. Boa, J. Rogez, Journal of Alloys and Compounds 520 (2012) 65Ð 71
B2617 - Highly active heteropolyanions supported Co catalysts for fast hydrogen generation in NaBH4 hydrolysis
This paper reports on the use of Co supported catalyst for the hydrolysis of NaBH4. Various materials with different acid/base surface properties have been chosen as supports (hydrotalcites, KF/Al2O3, heteropolyanions). The supports and the Co-containing catalysts were characterized by X-ray diffraction, scanning electron microscopy with energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, inductively coupled plasma, nitrogen adsorption. The NaBH4 hydrolysis reaction was studied in a liquid phase calorimeter coupled with a gas counter in order to follow at the same time the kinetics and the heat of reaction. Co supported on heteropolyanions showed great results in terms of reaction rate. Cobalt dispersed on heteropolyanions is a real promising catalytic system for the development of hydrogen generation in PEM fuel cells for portable devices.
Simona Bennici, Hao Yu, Emil Obeid, Aline Auroux, International Journal of Hydrogen Energy, 36 (2011) 7431Ð7442
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- May 14, 2012 - May 18, 2012
11th International Hydrocolloids Conference
Purdue University, USA11th International Hydrocolloids ConferenceBiofunctionality and Technofunctionality of Hydrocolloids14-18 May 2012, Whistler Center for Carbohydrate Research, Purdue University, USAThe 11th International Hydrocolloids Conference is organized by the world-renowned Whistler Center for Carbohydrate Research and will be held at The Stewart Center at Purdue University, Indiana, USA.
- April 30, 2012 - May 03, 2012
Carbon Capture Utilization & Sequestration
Pittsburgh, Pennsylvania - United States 11th Annual Conference on Carbon Capture Utilization & Sequestration April 30 - May 3, 2012Pittsburgh, Pennsylvania The 2012 Conference program follows in the footsteps of the past 10 events, with an added emphasis this year on potential utilization of anthropogenic carbon emissions that is reflected in the new name of the conference. The focus is on systems and technologies that are being or could be deployed in the U.S. and North America.
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