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E0073 - Thermoanalytical investigation of sodium acetate trihydrate for application as a latent heat thermal energy storage material
The thermal behaviour of sodium acetate trihydrate (NaAc. 3H20 ) was investigated by DTA, Q-TG and measurements of the solubility properties. The nucleation efficiency of Na4P207 9 10H20 for the crystallization of NaAc. 3H20 melts is not stable over lofig periods. Stratification can be ascribed to the formation of anhydrous sodium acetate in the supercooled melts. Under static heat storage conditions, NaAc- 3H20 and Na4P207 9 10H20 do not exhibit stable behaviour.
R. Naumann, Th. Fanghnel and H-H. Emons, Journal of Thermal Analysis 33 (1988) 685-688
E0072 - Evolution thermique d'un gel de borosilicate de plomb.
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W. Granier, K. Jabobker, M. Maurin, 16me JEEP (1990) 47-52
B2654 - Thermodynamic properties of pentalead tris(vanadate) chloride
In the present work the temperature dependences of pentalead tris(vanadate) chloride heat capacity have been measured for the first time in the range from 7 to 350 K. The experimental data were used to calculate standard thermodynamic functions, namely the heat capacity Cp ¡ (T), enthalpy H¡(T) ? H¡(0), entropy S¡(T) ? S¡(0) and Gibbs function G¡(T) ? H¡(0), for the range from T ? 0 to 350 K. The differential scanning calorimetry in temperature interval 298Ð1473 K was applied to measure temperatures of phase transition and melting of compound under study. The high-temperature X-ray diffraction in range 298Ð1073 K was used for the determining thermal expansion coefficients.
A.V. Knyazev, E.N. Bulanov, N.N. Smirnova, N.Yu. Kuznetsova, I.A. Letyanina, E.D. Pryamova, Thermochimica Acta 515 (2011) 79Ð83
B2653 - Separation of overlapping retained austenite decomposition and cementite precipitation reactions during tempering of martensitic steel by means of thermal analysis
During isochronal tempering of martensitic steels, several decomposition reactions take place within to some extent overlapping temperature regions. For the kinetic study of these reactions, differential scanning calorimetry and dilatometry are well established complementary experimental techniques. During tempering stages II and III of martensitic steels with increased carbon contents, the simultaneous transformation of retained austenite and the precipitation of cementite produce strong signals as well in the differential scanning calorimeter as in the dilatometer. For the determination of the individual kinetic parameters and reaction enthalpies, these reactions have to be separated, which is attempted in the present study. This is accomplished by tempering room temperature quenched as well as liquid nitrogen quenched specimens in a differential scanning calorimeter. The investigated material is the SAE 1070, a spring-steel with 10 vol% retained austenite after quenching to room temperature. The data evaluation procedure is explained in detail and the results are compared with literature data.
S. Primig, H. Leitner, Thermochimica Acta 526 (2011) 111Ð117
B2652 - Thermal decomposition kinetics of ammonium dinitramideÐguanylurea dinitramide mixture analyzed by isoconversional methods
The thermal decomposition kinetics of a mixture of high-energy oxidizers ammonium dinitramide (ADN) and guanylurea dinitramide (GUDN) have been studied by nonisothermal differential scanning calorimetry (DSC). Friedman's and Vyazovkin's advanced isoconversional (AIC-V) methods were used to investigate the dependence of activation energy (Ea) on conversion (?). A strong dependence of Ea on ? was observed, indicating a complex decomposition process. Ea is ?165Ð175 kJ mol?1 at the start of the reaction, then reaches a maximum of ?196Ð199 kJ mol?1 at ? = ?0.4, followed by a strong decrease to ?135 kJ mol?1 near the end. Ea has also been determined for the mixture and the individual components using Kissinger's method. Our results suggest that the decomposition of ADN greatly influences the observed Ea dependence on ?. This is further supported by Fourier transform infrared (FTIR) results and the enthalpy values of exothermic decomposition.
G. Santhosh, Robbin Poh Cheng Tien, Ang How Ghee, Thermochimica Acta 480 (2008) 43Ð48
B2651 - Crystal structure and thermodynamic properties of potassium antimony tungsten oxide
In the present work potassium antimony tungsten oxide with pyrochlore structure is refined by the Rietveld method (space group Fd3m, Z = 8). The temperature dependences of heat capacity have been measured for the first time in the range from 7 to 370 K for this compound. The experimental data were used to calculate standard thermodynamic functions, namely the heat capacity , enthalpy H¡(T) ? H¡(0), entropy S¡(T) ? S¡(0) and Gibbs function G¡(T) ? H¡(0), for the range from T ? 0 to 370 K. The differential scanning calorimetry was applied to measure the incongruent melting temperature of compound under study. The high-temperature X-ray diffraction was used for the determining thermal expansion coefficients.
Aleksandr V. Knyazev, Ivan G. Tananaev, Nataliya Yu. Kuznetsova, Nataliya N. Smirnova, Irene A. Letyanina, Igor V. Ladenkov, Thermochimica Acta 499 (2010) 155Ð159
B2650 - Nucleation Barriers for the Liquid-To-Crystal Transition in Ni: Experiment and Simulation
Nucleation in undercooled Ni is investigated by a combination of differential scanning calorimetry (DSC) experiments and Monte Carlo (MC) simulation. By systematically varying the sample size in the DSC experiments, nucleation rates J over a range of 8 orders of magnitude are obtained. Evidence is given that these rates correspond to homogeneous nucleation. Free energy barriers G , as extracted from the measured J, are in very good agreement with those from the MC simulation. The MC simulation indicates a nonspherical geometry of crystalline clusters, fluctuating between prolate and oblate shape at a given size. Nevertheless, the temperature dependence of G is well described by classical nucleation theory.
J. Bokeloh, R. E. Rozas, J. Horbach, G. Wilde, Physical Review Letter 107, 145701 (2011)
B2649 - Metabolic depression in fish measured by direct calorimetry: A review
In nature under adverse conditions like low oxygen conditions or starvation fish often lower their metabolism: Ômetabolic depressionÕ. This strategy of lowering the metabolic rate is a survival strategy and is used to save energy stores and diminish end-product accumulation. The overall metabolic rate of animals can be deduced by measuring metabolic processes such as oxygen consumption, but the ultimate method is measuring heat flow. In this review, we will summarise the available data about metabolic depression measuring heat flow, i.e. by direct calorimetry in fishes, which were carried out almost exclusively with a 1-l flow through calorimeter. Using deconvolution techniques the time constant of this calorimeter was measured that allowed to estimate the time course of metabolic depression, which was found to take place on a time scale of 20Ð30 min. We demonstrated that metabolic depression is species dependent. Goldfish, eel and tilapia show metabolic depression under low oxygen conditions while this is not the case for common carp. In addition it is shown that metabolic depression is flexible and increases with decreasing oxygen availability. Furthermore using a video analysing system we demonstrated that metabolic depression is not caused by a reduction of external activity. As heart rate falls dramatically during metabolic depression as shown by small wireless transmitters, we hypothesise that blood flow reduction might be the proximate cause for metabolic depression.
Vincent van Ginneken, Guido van den Thillart, Thermochimica Acta, 483 (2009) 1Ð7
B2648 - Calorimetric Measurement of Surface and Interface Enthalpies of Yttria-Stabilized Zirconia (YSZ)
The surface and interface enthalpies of cubic stabilized zirconia solid solutions containing 8, 10, and 12 mol?% Y2O3 were determined by a combination of calorimetric, morphological, and structural analyses techniques. Nanocrystalline samples with several surface areas and degrees of agglomeration were synthesized by simultaneous precipitation and annealing at temperatures of 470?900 ¡C. Samples were characterized by X-ray diffraction and Raman spectroscopy. Surface areas were measured by N2 adsorption, and interface areas were estimated by comparing surface areas from N2 adsorption to those derived from an analysis of the crystallite sizes refined from X-ray diffraction data. Calorimetric measurements of heat of solution in a sodium molybdate melt, as a function of surface and interface areas, enabled us to experimentally derive trends in the surface and interface enthalpies of hydroxylated surfaces. Accounting for heats of water adsorption measured by microcalorimetry allowed us to obtain the surface enthalpies (energies) of the anhydrous surfaces at each composition. Average surface enthalpies were determined to increase with yttria content, from 0.85 ± 0.07 J/m2 (for 8 mol?% yttria) to 1.27 ± 0.08 J/m2 (for 12 mol?% yttria) for the hydrous surface and from 1.16 ± 0.08 J/m2 to 1.80 ± 0.10 J/m2 for the anhydrous surface. Interface enthalpies were determined to be in the range of 0.9 ± 0.5 J/m2 for all studied compositions. Comparisons with measured surface energies for pure ZrO2, and Y2O3 nanopowders and grain-boundary energies for YSZ dense nanoceramics are presented.
Gustavo C. C. Costa, Sergey V. Ushakov, Ricardo H. R. Castro, Alexandra Navrotsky, Reginaldo Muccillo, Chem. Mater., 2010, 22 (9) 2937Ð2945
B2647 - Thermochemistry of proton containing borosilicate, aluminosilicate and gallosilicate zeolite beta
The thermochemistry of proton containing borosilicate, aluminosilicate and gallosilicate zeolites with beta topology (B-BEA, Al-BEA and Ga-BEA) is described. Thermogravimetry and differential scanning calorimetry on these materials indicate the substitution of Al by Ga or B in the beta framework reduces the decomposition temperature. Water adsorption calorimetry directly measured the hydration enthalpies of these samples. B-BEA and Ga-BEA have less exothermic hydration enthalpies than Al-BEA. High temperature oxide melt solution calorimetry was performed to derive the formation enthalpies of hydrated samples (8.9Ð18.8 kJ/mol relative to oxides on TO2 molar basis). The formation enthalpies of dehydrated phases (33.2Ð55.1 kJ/mol relative to oxides on TO2 molar basis) were calculated from the formation enthalpies of hydrated phases and the hydration enthalpy.
Wei Zhou, Pingping Sun, Peng Zhang, Alexandra Navrotsky, Microporous and Mesoporous Materials, 142 (2011) 749Ð753
B2646 - Structure and Energetics of a New Hydrate of 4?-Hydroxyacetophenone
A new hydrate of 4?-hydroxyacetophenone (HAP), triclinic, space group P1?, was isolated and characterized. Both the structure determination by single crystal X-ray diffraction at 150 K and the results of thermogravimetry analysis carried out in the temperature range 263?363 K indicated the H2O/HAP molar ratio to be 1.5. The water molecules line up in chains that reside in lattice channels (channel hydrate) and are sustained by OHáááO hydrogen bonds. The chains also interact with the OH (donor) and CO (acceptor) groups of the HAP molecules through OHáááO hydrogen bonds. The results suggest that the OH and CH3CO groups of the HAP molecules in the hydrate are in a syn orientation. This conformation is the same as that observed for the previously described anhydrous form II (orthorhombic, P212121). The dehydration process generates, however, the form I HAP polymorph (monoclinic, P21/c), where the anti conformation is preferred. From drop-sublimation Calvet microcalorimetry experiments it was possible to conclude that ?f H¡m(HAPá1.5H2O, cr) = ?812.5 ± 3.1 kJámol?1, at 298.15 K. Finally, thermodynamic analysis of the temperature and relative humidity effects on the dehydration process to yield HAP(cr I) and H2O(g) indicated that loss of water becomes favorable (?rGm < 0) at 298.15 K, for a relative humidity of 66%. This value is compatible with routine laboratory observations of the HAPá1.5H2O(cr) stability at ambient temperature. The analysis also suggested that, independently of the relative humidity, the hydrate will tend to decompose above 331 K, a temperature that closely matches the high limit of the dehydration range observed in the TG experiments.
Carlos E. S. Bernardes, M. Fa?tima M. Piedade, Manuel E. Minas da Piedade, Cryst. Growth Des., 2010, 10 (7), 3070Ð3076
B2645 - n-Butane adsorption on Cu3(btc)2 and MIL-101
The n-butane adsorption capacity and heat of adsorption for the metalÐorganic frameworks Cu3(btc)2 (btc = benzene-1,3,5-tricarboxylate) and MIL-101 was determined at three different temperatures (293, 303, and 313 K) under dynamic conditions at atmospheric pressure with a micro-balance combined with a Tian-Calvet micro-calorimeter. The adsorption rate was studied at the adsorption temperature of 293 K. The n-butane adsorption properties were compared with activated carbon Sorbonorit 3. For low n-butane concentration the microporous Cu3(btc)2 has a higher storage capacity than the mesoporous material MIL-101. For high n-butane concentrations it is vice versa. The saturation capacity at 293 K for Cu3(btc)2 is 3.7 mmol g?1 and for MIL-101 remarkable 11.2 mmol g?1. The storage capacity and adsorption rate depends on the alkane concentration. For higher n-butane concentration MIL-101 has a higher adsorption rate than Cu3(btc)2 independent on the amount of adsorbed n-butane
Nicole Klein, Antje Henschel, Stefan Kaskel, Microporous and Mesoporous Materials, 129 (2010) 238Ð242
B2644 - Enthalpies of formation of NbÐRu and NbÐRuÐAl alloys
The enthalpies of formation of NbÐRu alloys in the whole range of composition and of two compositions in the NbÐRuÐAl ternary system corresponding to Nb(Ru,Al)2 and NbRu2Al identified by Cerba et al. [P. Cerba, M. Vilasi, B. Malaman, J. Steinmetz, J. Alloys Compd. 201 (1993), 57Ð60], have been measured by high-temperature direct reaction synthesis calorimetry at 1775 K. For some binary alloys the experiment cannot provide results because the direct reaction synthesis is not completed contrarily to ternary alloys experiments. The results are compared with predicted ab initio data.
My.Y. Benarchid, N. David, J.-M. Fiorani, M. Vilasi, T. Benlaharche, Thermochimica Acta, 482 (2009) 39Ð41
B2643 - Enthalpies of formation of MoÐRu and MoÐRuÐSi compounds determined by high-temperature direct reaction synthesis calorimetry
The enthalpies of formation of (Ru) hcp solid solution and Mo5Ru3 (? phase) in the MoÐRu system and ternary extension in the MoÐRuÐSi system at Mo56Ru37Si7 composition, have been determined by high-temperature direct reaction synthesis calorimetry at 1760 K. The following values are reported: ?fH1760 K(Ru) = ?10.6 ± 0.5 kJ/mol at.%; ?fH1760 K(Mo5Ru3) = ?7.4 ± 0.4 kJ/mol at.%; ?fH1760 K(Mo56Ru37Si7) = ?13.1 ± 3.3 kJ/mol at.%. The results are compared with the previous values derived from e.m.f. measurements. They are also compared with the predicted values obtained by Calphad, by ab initio method combined to Calphad modelling, and derived from a thermodynamic database named ÒTM16.TDBÓ.
My. Y. Benarchid, N. David, J.-M. Fiorani, M. Vilasi, Thermochimica Acta, 494 (2009) 26Ð29
B2642 - Non-isothermal crystallization kinetic of poly(ethylene terephthalate)/fumed silica (PET/SiO2) prepared by in situ polymerization
A number of poly(ethylene terephthalate) (PET) nanocomposites were prepared by in situ polymerization using different amounts (0.5, 1, 2, 3 and 4 wt%) of fumed silica (SiO2). The polymerization of PET was carried out by the two-stage melt polycondensation method. From DSC studies it was found that the melting point of the nanocomposites was shifted slightly to higher temperatures by the addition of SiO2 till 3 wt% while for PETÐ4 wt% SiO2 nanocomposite the melting point was reduced. As the amount of SiO2 was increased the crystallization became faster, and there was, also, a shifting of the temperature of the crystallization peak to higher values, this being evidence that SiO2 can act as nucleating agent. At higher content (3 and 4 wt%) the temperature of the crystallization peak is lower than that of PETÐ2 wt% SiO2 due to the formation of crosslinked macromolecules. The activation energy is calculated with the Friedman's method. PET/SiO2 samples present lower activation energy compared to that of neat PET, except those of PETÐ4% SiO2, in which the activation energy have a maximum value for ? = 0.8 probably due to the second crystallization peak. Extensive crystallization studies by using Avrami, Ozawa and Malek methods verified that PET and its nanocomposites must be crystallized by two mechanisms with different activation energies taking place in different degrees of crystallization.
G. Antoniadis, K.M. Paraskevopoulos, D. Bikiaris, K. Chrissafis, Thermochimica Acta, 510 (2010) 103Ð112
B2641 - Kinetics study of cold-crystallization of poly(ethylene terephthalate) nanocomposites with multi-walled carbon nanotubes
A series of PET/MWCNTs nanocomposites were prepared by in situ polymerization using different amounts of multi-walled carbon nanotubes (MWCNTs). The polymerization of poly(ethylene terephthalate) (PET) was prepared by the two-stage melt polycondensation method. The values of the activation energy of the nanocomposites, as calculated with the Kissinger's and OzawaÐFlynnÐWall (OFW) methods, are larger than the ones of pristine PET. These values are 107.9 kJ/mol for PET-0% MWCNTs and 154.0 kJ/mol for PET-1% MWCNTs which is the larger value among all. Avrami plots present a linear portion, almost parallel to each other, which is followed by a deviation at larger temperatures. Straight lines are obtained from Ozawa plots only for PET-0.25% MWCNTs at least for three different heating rates. The dependence of the activation energy on the degree of conversion, from the Avrami, Malek and Ozawa plots, gives indications that for the kinetic description of the cold-crystallization of PET/MWCNTs cannot be used only one crystallization mechanism which obeys to Avrami equation. Only for the PET-0.25 one crystallization mechanism can be used at least for the major part of the crystallization conversion. So, in order to describe their crystallization mechanisms at least two mechanisms with different activation energies must be used. These two mechanisms maybe are taking part in different degree of crystallization conversions for every nanocomposite.
G. Antoniadis, K.M. Paraskevopoulos, D. Bikiaris, K. Chrissafis, Thermochimica Acta,493 (2009) 68Ð75
B2640 - Specific heats of ternary oxides in the LiÐU(VI)ÐO System
Seven ternary oxides; Li4UO5, Li2UO4, Li22U18O65, Li2U1.75O6.25, Li2U2O7, Li2U3O10 and Li2U6O19 in the system LiÐU(VI)ÐO were prepared by solid-state reaction route and characterized by X-ray diffraction method. Specific heats of these compounds were measured by differential scanning calorimetry in the temperature range from 300 to 860 K. The specific heats show a decreasing trend with increase in UO3(s) content in these lithium uranates. However, the specific heat per gram atom shows an increasing trend with decrease in number of oxygen atoms in the formula unit.
S.K. Rakshit, Ram Avtar Jat, Y.P. Naik, S.C. Parida, Ziley Singh, B.K. Sen, Thermochimica Acta, 490 (2009) 60Ð63
B2639 - Combined experimental and computational study on the energetics of 1,2-benzisothiazol-3(2H)-one and 1,4-benzothiazin-3(2H, 4H)-one
The present work reports an experimental and computational study of the energetics of 1,2-benzisothiazol-3(2H)-one and 1,4-benzothiazin-3(2H, 4H)-one. The standard (p¡ = 0.1 MPa) massic energy of combustion, at T = 298.15 K, of each compound was measured by rotating bomb combustion calorimetry, in oxygen that allowed the calculation of the respective standard molar enthalpy of formation, in the condensed phase, at T = 298.15 K. The standard molar enthalpies of sublimation, at T = 298.15 K, were measured by high-temperature Calvet microcalorimetry. From the combination of data obtained by both techniques we have calculated the standard molar enthalpies of formation, in the gaseous phase, at T = 298.15 K. In addition, computational calculations were carried using the density functional theory with the B3LYP functional and the 6-31G? basis set and some correlations between structure and energetics were obtained for the keto and enol forms of both compounds. Using the G3(MP2)//B3LYP composite method and various appropriate reactions, the standard molar enthalpies of formation of 1,2-benzisothiazol-3(2H)-one and 1,4-benzothiazin-3(2H, 4H)-one, at T = 298.15 K, were computationally derived and compared with the experimental data. The aromaticity of 1,2-benzisothiazol-3(2H)-one, 1,4-benzothiazin-3(2H, 4H)-one and that of some related species was evaluated by analysis of nucleus independent chemical shifts (NICS).
Margarida S. Miranda, M. Agostinha R. Matos, Victor M.F. Morais, Joel F. Liebman, The Journal of Chemical Thermodynamics, 43 (2011) 635Ð644
B2638 - Thermodynamic study of phase transitions of imidazoles and 1-methylimidazoles
The vapor pressures of imidazole, N-methylimidazole and of their dichloro and dicyano substituted compounds were measured at different temperatures, in the crystalline phase for two of them, and in crystalline and liquid phases for the other four. From these measurements, enthalpies and standard entropies of sublimation and vaporization were derived. The results allowed the determination of the triple points (p, T) coordinates of the four compounds studied in both condensed phases as well as the calculation of their enthalpy of fusion. Enthalpies and temperatures of fusion were also determined using d.s.c. The experimental results enabled the estimation of the enthalpy of the intermolecular NÐH?N bonds in the imidazoles studied.
Ana R.R.P. Almeida, Manuel J.S. Monte, The Journal of Chemical Thermodynamics, 44 (2012) 163Ð168
B2637 - Fluorene: An extended experimental thermodynamic study
This work reports new experimental thermodynamic results on fluorene. Vapor pressures of both crystalline and liquid phases were measured using a pressure gauge (capacitance diaphragm manometer) and Knudsen effusion methods over a wide temperature range (292.20 to 412.16) K yielding accurate determination of enthalpy and entropy of sublimation and of vaporization. The enthalpy of sublimation was also determined using Calvet microcalorimetry. The enthalpy of fusion was derived from vapor pressure results and from d.s.c. experiments. Static bomb calorimetry was used to determine the enthalpy of combustion of fluorene from which the standard enthalpy of formation in the crystalline phase was calculated. The enthalpy of formation in the gaseous phase was calculated combining the result derived for the crystalline phase with the enthalpy of sublimation.
ManuelJ.S. Monte, S--nia P. Pinto, Ana I.M.C. Lobo Ferreira, Lu'sa M.P.F. Amaral, Vera L.S. Freitas, Maria D.M.C. Ribeiro da Silva, The Journal of Chemical Thermodynamics, 45 (2012) 53Ð58
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- 16 Mai 2012 - 18 Mai 2012
INNOSTOCK 2012
Lleida, SpainINNOSTOCK 2012The 12th International Conference on Energy Storage16-18 May 2012Innostock 2012 is part of the Stock conference series sponsored by the ECES IA of the International Energy Agency.Innostock 2012 will gather the world’s leading specialists and academic researchers within the field of energy efficiency through energy storage. Energy storage will present in all its topics:• Underground thermal energy storage• Sensible, latent and thermochemical energy storage• Electrical storage
- 14 Mai 2012 - 18 Mai 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.
- 30 Avril 2012 - 03 Mai 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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