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B2456 - Dehydrated native biopolymers Ð a unique representative of glassy systems
The present work summarizes the results of our studies of the heat induced conformational and relaxation transitions in all the three main classes of biopolymers at different hydration degree. Detection of the excess heat capacity drop and absolute values of the heat capacity in a wide range of temperatures and water content allowed us to get a deeper insight in the nature of the processes occurring in these biopolymers. As a result, we were able to distinguish the individual features of the thermal properties related to the peculiarities of the steric structure for each biopolymer studied and assess common features for every biopolymer system undergoing a glass transition.
G. I. Tsereteli, T. V. Belopolskaya, N. A. Grunina, Journal of Thermal Analysis and Calorimetry, Vol. 92 (2008) 3, 711Ð716
B2455 - Low-temperature heat capacities and thermodynamic properties of 2,2-dimethyl-1,3-propanediol
The molar heat capacities Cp,m of 2,2-dimethyl-1,3-propanediol were measured in the temperature range from 78 to 410 K by means of a small sample automated adiabatic calorimeter. A solidÐsolid and a solidÐliquid phase transitions were found at T=314.304 and 402.402 K, respectively, from the experimental CpÐT curve. The molar enthalpies and entropies of these transitions were determined to be 14.78 kJ molÐ1, 47.01 J KÐ1 molÐ1 for the solid-solid transition and 7.518 kJ molÐ1, 18.68 J KÐ1 molÐ1 for the solidÐliquid transition, respectively. The dependence of heat capacity on the temperature was fitted to the following polynomial equations with least square method. In the temperature range of 80 to 310 K, Cp,m/(J KÐ1 molÐ1)=117.72+58.8022x+3.0964x2 + 6.87363x3Ð13.922x4+9.8889x5+16.195x6; x=[(T/K)Ð195]/115. In the temperature range of 325 to 395 K, Cp,m/(J KÐ1 molÐ1)= 290.74+22.767xÐ0.6247x2Ð0.8716x3Ð4.0159x4Ð0.2878x5+1.7244x6; x=[(T/K)Ð360]/35. The thermodynamic functions HTÐH298.15 and STÐS298.15, were derived from the heat capacity data in the temperature range of 80 to 410 K with an interval of 5 K. The thermostablility of the compound was further tested by DSC and TG measurements. The results were in agreement with those obtained by adiabatic calorimetry.
B. Tong, Z.-C. Tan, X. C. Lv, L. X. Sun, F. Xu, Q. Shi, Y. S. Li, Journal of Thermal Analysis and Calorimetry, Vol. 90 (2007) 1, 217Ð221
B2454 - Phase diagram of palmitic acid-tetradecanol mixtures obtained by DSC experiments
A series of PAÐTD mixtures were prepared and their thermal properties were studied by DSC and thermal conductivity measurement. The phase diagram of the binary system was constructed, which showed an eutectic behavior for the solidÐliquid equilibrium line. The eutectic composition of the binary system was at the mass fraction of TD near 0.7 with an eutectic temperature of about 29¡C. At TD side, PA was partially miscible in the TD solid matrix and the solid phase transition of TD had an effect on the solidus line. The eutectic composition mixture could be viewed as a new phase change material with large thermal energy storage capacity.
J. L. Zeng, Z. Cao, D. W. Yang, F. Xu, L. X. Sun, L. Zhang, X. F. Zhang, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 2, 501Ð505
B2453 - Molar heat capacity and thermodynamic properties of crystalline Ho(Asp)Cl2,6H2O
The molar heat capacity, Cp,m, of a complex of holmium chloride coordinated with L-aspartic acid, Ho(Asp)Cl2á6H2O, was measured from 80 to 397 K with an automated adiabatic calorimeter. The thermodynamic functions HTÐH298.15 and STÐS298.15 were derived from 80 to 395 K with temperature interval of 5 K. The thermal stability of the complex was investigated by differential scanning calorimeter (DSC) and thermogravimetric (TG) technique, and the mechanism of thermal decomposing of the complex was determined based on the structure and the thermal analysis experiment.
B. P. Liu, X. C. Lv, Z. C. Tan, Z. H. Zhang, Q. Shi, L. N. Yang, J. Xing, L. X. Sun, T. Zhang, Journal of Thermal Analysis and Calorimetry, Vol. 89 (2007) 1, 283Ð287
B2452 - Gelled Na2HPO4 12H2O with amylose-g-sodium acrylate: heat storage performance, heat capacity and heat of fusion
A novel gelling method was studied to stabilize phase change material Na2HPO4,12H2O with amylose grafted sodium acrylate. Gelled Na2HPO4,12H2O shows stable heat storage performance prepared at optimized conditions: 2.7mass/mass% sodium acrylate, 0.4 mass/mass% amylose, 0.05Ð0.09 mass/mass% N, N0-methylene-bisacrylamide, 0.05Ð0.09 mass/mass% K2S2O8 and Na2SO3 (mass ratio 1:1), at 50 ¡C. Na2HPO4,12H2O was dispersed in gel network as tiny crystals less than 0.1 mm. Melting points were in the range 35.4 ± 2 ¡C. Short-term thermal cycling proves the effectiveness of the novel method for eliminating phase separation in the gelled salt. Adiabatic calorimetric measurement of heat capacities shows two phase transitions, which correspond to melting of Na2HPO4 12H2O and freezable bond water in gel, respectively. Heat of fusion of pure Na2HPO4,12H2O was determined as 260.9 J g-1. Distribution of extra water is: free water:freezable water:nonfreezing water = 0:0.85:0.15.
X.-Z. Lan, Z.-C. Tan, Q. Shi, Z.-H. Gao, J Therm Anal Calorim (2009) 96:1035Ð1040
B2451 - Low-temperature heat capacity and thermodynamic properties of crystalline lead formate
As one 3-D coordination polymer, lead formate was synthesized; calorimetric study and thermal analysis for this compound were performed. The low-temperature heat capacity of lead formate was measured by a precise automated adiabatic calorimeter over the temperature range from 80 to 380 K. No thermal anomaly or phase transition was observed in this temperature range. A four-step sequential thermal decomposition mechanism for the lead formate was found through the DSC and TG-DTG techniques at the temperature range from 500 to 635 K.
J. Zhang, Y. Y. Liu, Z. H. Zhang, X. C. Lv, L. X. Sun, F. Xu, Z. C. Tan, T. Zhang, Y. Sawada, Journal of Thermal Analysis and Calorimetry, Vol. 89 (2007) 2, 643Ð647
B2450 - Mechanism and kinetics of the formation of zinc pack coatings
A zinc deposition method that could be used instead hot-dip galvanizing is pack cementation, where the substrate is heated immersed in a powder mixture containing Zn and a halide activator (NH4Cl). In the present work the mechanism of this process is examined, along with the effect of temperature and heating time on the coating thickness and structure. For this purpose the coating was deposited and characterized with SEM, while the deposition mechanism was investigated with DSC. From the above examination it was deduced that the deposition of Zn takes place with a multiple-step mechanism, which involves several reactions in the gaseous phase including the formation of volatile zinc halides and finally the diffusion of zinc in the crystal lattice of the ferrous substrate. This procedure is accomplished at about 300¡C and leads to the growth of a coating composed by two layers referring to and phase of the FeÐZn system. The coating deposition rate seems to be controlled by the zinc diffusion as its determination at 300 and 350¡C showed, where it was deduced that the coating thickness is a linear function of the square root of heating time. However the coating structure is not affected by the heating time and temperature
G. Vourlias, N. Pistofidis, K. Chrissafis, E. Pavlidou, G. Stergioudis, Journal of Thermal Analysis and Calorimetry, Vol. 91 (2008) 2, 497Ð501
B2449 - Role of structural and macrocrystalline factors in the desolvation behaviour of cortisone acetate solvates
A combined analysis of structural data and experimental results (DSC, temperature-resolved XRPD and hot stage optical microscopy) revealed that the dehydration mechanism of cortisone acetate monohydrate (CTAáH2O) involves a collective and anisotropic departure of water molecules followed by a cooperative structural reorganization toward the anhydrous polymorph CTA (form 2). In spite of the lack of crystal structure data, it can be postulated from experimental data that thermal decomposition of the dihydrated form (CTAá2H2O) and of the tetrahydrofuran solvate (CTAáTHF) toward another polymorph (CTA (form 3)) also proceeds according to a cooperative mechanism, thus giving rise to probable structural filiations between these crystalline forms of CTA. The crystal structure determination of two original solvates (CTAáDMF and CTAáDMSO) indicates that these phases are isomorphous to the previously reported acetone solvate. However, their desolvation behaviour does not involve a cooperative mechanism, as could be expected from structural data only. Instead, the decomposition mechanism of CTAáDMF and CTAáDMSO starts with the formation of a solvent-proof superficial layer, followed by the partial dissolution of the enclosed inner part of crystals. Hot stage optical microscopy observations and DSC measurements showed that dissolved materials (resulting from a peritectic decomposition) is suddenly evacuated through macroscopic cracks about 30¡C above the ebullition point of each solvent. From this unusual behaviour, the necessity to investigate rigorously the various aspects (thermodynamics, kinetics, crystal structures and physical factors) of solvate decompositions is highlighted, including factors related to the particular preparation route of each sample.
S. Petit, F. Mallet, M.-N. Petit, G. Coquerel, Journal of Thermal Analysis and Calorimetry, Vol. 90 (2007) 1, 39Ð47
B2448 - Mesophase formation and thermal behavior of catanionic mixtures of gemini surfactants with sodium alkylsulfates
The thermal behavior for three homologous series of cationic geminis surfactants of the type n-2-n, alkanediyl-a,x-bis(alkyldimethylammonium bromide), with n = 12, 14, 16, and 18, and sodium alkyl sulfates, SCmS, with m = 12, 14, and 16, is reported here. The cationic/anionic molar ratio is kept at 1:2 (equicharged mixtures), and salt is also present. Polarizing light microscopy and differential scanning calorimetry show a stepwise fusion for the mixtures with appearance of several mesophases between the crystalline structures and the isotropic liquid. A main endothermic transition is observed, associated with partial chain melting and consequent loss of crystalline order, followed by a transition to a smectic liquid crystal. The phase transition thermodynamics is interpreted in terms of an interplay between van der Waals chainÐchain interactions and ionic head group interactions.
Yujie Wang, Eduardo F. Marques, J Therm Anal Calorim (2010) 100:501Ð508
B2447 - Energetics of lead(II), cadmium(II) and zinc(II) complexes with amino acids
The molar heat capacity and the standard (p0 = 0.1 MPa) molar enthalpies of formation of the crystalline of bis(glycinate)lead(II), Pb(gly)2; bis(DL-alaninate) lead(II), Pb(DL-ala)2; bis(DL-valinate)lead(II), Pb(DL-val)2, bis(DL-valinate)cadmium(II), Cd(DL-val)2 and bis(DL-valinate) zinc(II), Zn(DL-val)2, were determined, at T = 298.15 K, by differential scanning calorimetry, and high precision solution-reaction calorimetry, respectively. The standard molar enthalpies of formation of the complexes in the gaseous state, the mean molar metalÐligand dissociation enthalpies, M(II)Ðamino acid, hDmi(MÐL), were derived and compared with analogous copper(II)Ðligand and nickel(II)Ðligand.
Manuel A. V. Ribeiro da Silva, Luõs M. N. B. F. Santos, Ana C. P. Faria, Filipa S. A. Sistelo, J Therm Anal Calorim (2010) 100:475Ð482
B2446 - Thermodynamic investigation of several natural polyols. Part III. Heat capacities and thermodynamic properties of erythritol
The low-temperature heat capacity Cp,m of erythritol (C4H10O4, CAS 149-32-6) was precisely measured in the temperature range from 80 to 410 K by means of a small sample automated adiabatic calorimeter. A solidÐliquid phase transition was found at T=390.254 K from the experimental CpÐT curve. The molar enthalpy and entropy of this transition were determined to be 37.92±0.19 kJ molÐ1 and 97.17±0.49 J KÐ1 molÐ1, respectively. The thermodynamic functions [HTÐH298.15] and [STÐS298.15], were derived from the heat capacity data in the temperature range of 80 to 410 K with an interval of 5 K. The standard molar enthalpy of combustion and the standard molar enthalpy of formation of the compound have been determined: ?c Hmo (C4H10O4, cr)= Ð2102.90±1.56 kJ molÐ1 and ?f Hmo (C4H10O4, cr)= Ð 900.29±0.84 kJ molÐ1, by means of a precision oxygen-bomb combustion calorimeter at T=298.15 K. DSC and TG measurements were performed to study the thermostability of the compound. The results were in agreement with those obtained from heat capacity measurements.
B. Tong, Z. C. Tan, J. N. Zhang, S. X. Wang, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 2, 469Ð475
B2445 - Thermal stability evaluation of doping compounds before GC-MS analysis by DSC
The Medical Commission of the International Olympic Committee forbids the use of anabolic androgenic steroids, b-agonists, stimulant and narcotic compounds to improve athletic performance. In this work, we evaluated the thermal stability of 17 compounds by the use of the DSC for their potential GC-MS analysis either under free form or under TMS derivative form. In DSC, esterified and unesterified anabolic steroids were characterized by a true melting peak, followed by a large exothermic peak at about 251Ð316¡C due to oxidative degradation. They could be analysed by GC-MS mainly under TMS derivatives. Hydroxylated and unhydroxylated stimulant compounds (xanthines) seemed to be more stable at high temperature. As unhydroxylated xanthines were not silylated with BSTFA Ð TMCS, their GC analysis would be done under their free forms. TMS derivatisation of albuterol hemisulfate and codeine phosphate is preferable. In our conditions, to analyse by GC-MS all 17 doping compounds in the same GC-MS run, the optimal silylation temperature and best column initial temperature were determined at both 60¡C.
Y. Hadef, J. Kaloustian, A. Nicolay, H. Portugal, Journal of Thermal Analysis and Calorimetry, Vol. 93 (2008) 2, 553Ð560
B2444 - Dissociation Enthalpies of Synthesized Multicomponent Gas Hydrates with Respect to the Guest Composition and Cage Occupancy
This study presents the influences of additional guest molecules such as C2H6, C3H8, and CO2 on methane hydrates regarding their thermal behavior. For this purpose, the onset temperatures of decomposition as well as the enthalpies of dissociation were determined for synthesized multicomponent gas hydrates in the range of 173-290 K at atmospheric pressure using a Calvet heat-flow calorimeter. Furthermore, the structures and the compositions of the hydrates were obtained using X-ray diffraction and Raman spectroscopy as well as hydrate prediction program calculations. It is shown that the onset temperature of decomposition of both sI and sII hydrates tends to increase with an increasing number of larger guest molecules than methane occupying the large cavities. The results of the calorimetric measurements also indicate that the molar dissociation enthalpy depends on the guest-to-cavity size ratio and the actual concentration of the guest occupying the large cavities of the hydrate. To our knowledge, this is the first study that observes this behavior using calorimetrical measurements on mixed gas hydrates at these temperature and pressure conditions
Marisa B. Rydzy, Judith M. Schicks, Rudolf Naumann, Jrg Erzinger, J. Phys. Chem. B 2007, 111, 9539-9545
B2443 - Thermodynamic properties of uranium plutonium mixed carbides
High plutonium containing hyperstoichiometric mixed carbide fuels are used as driver fuel in the Fast Breeder Test Reactor at Kalpakkam, India. The enthalpy increment of the mixed carbide fuels were measured in the temperature range 1000Ð1800 K using a high temperature drop calorimeter. The results are presented and compared with the data available in the literature.
R. Kandan, R. Babu, K. Nagarajan, J Therm Anal Calorim (2010) 99:713Ð717
B2442 - Calorimetric investigations on stoichiometric barium and uranium oxides
Heat capacities and enthalpy increments of barium uranates: BaU2O7(s), Ba2U3O11(s), Ba2.875UO5.875(s) and Ba3UO6(s) were measured using a differential scanning calorimeter and a high-temperature Calvet calorimeter. The heat capacities and enthalpy increments were measured in the temperature range 126Ð304 K and 299Ð1011 K, respectively. A set of self consistent thermodynamic functions such as entropy, Gibbs energy function, heat capacity and Gibbs energy and enthalpy of formation values for BaU2O7(s), Ba2U3O11(s), Ba2.875UO5.875(s) and Ba3UO6(s) have been computed for the first time using the data obtained in the present study and other available experimental data.
Smruti Dash, Ziley Singh, Journal of Nuclear Materials 404 (2010) 9Ð18
B2441 - Thermochemistry of paracetamol
Combustion calorimetry, Calvet-drop sublimation calorimetry, and the Knudsen effusion method were used to determine the standard (Po = 0.1 MPa) molar enthalpies of formation of monoclinic (form I) and gaseous paracetamol, at T = 298.15 K.
Ricardo Picciochi, Hermõnio P. Diogo, Manuel E. Minas da Piedade, J Therm Anal Calorim (2010) 100:391Ð401
B2440 - Energetic studies of two oxygen heterocyclic compounds: Xanthone and tetrahydro-c-pyrone
The present work reports an experimental thermochemical study supported by state of the art calculations of two heterocyclic compounds containing oxygen in the ring: xanthone and tetrahydro-c-pyrone. The standard (Po = 0.1 MPa) molar enthalpies of formation in the condensed phase, at T = 298.15 K, were derived from the measurements of the standard molar energies of combustion in oxygen atmosphere, using a static bomb calorimeter. The standard molar enthalpies of sublimation or vaporization, at T = 298.15 K, of the title compounds were obtained from Calvet microcalorimetry measurements. These values were used to derive the standard enthalpies of formation of the compounds in the gas-phase at the same temperature, which were compared with estimated data from G3(MP2)//B3LYP computations.
Vera L. S. Freitas, Jose R. B. Gomes, Maria D. M. C. Ribeiro da Silva, J Therm Anal Calorim (2009) 97:827Ð833
B2439 - Energetics of some sulphur heterocycles. Thiophene derivatives
The present work is part of a broader research program on the energetics of formation of heterocycles, aiming the study of the enthalpic effects of the introduction of different substituents into heterocycles. In this work we present the results of the thermochemical research on sulphur heterocycles of the type substituted thiophenes with different kind of substituents, mainly alkyl, ester, acetyl, carboxamide, acetamide, carbonitrile and carboxaldehyde. The standard (p¡=0.1MPa) molar enthalpies of formation, in the condensed phase, at T=298.15 K, of a large number of substituted thiophenes, were derived from their standard massic energies of combustion, measured by rotating-bomb combustion calorimetry, while the standard molar enthalpies of vaporization or sublimation of those compounds were obtained either by high temperature Calvet Microcalorimetry, or by the temperature dependence of their vapour pressures determined by the Knudsen effusion technique. The standard molar enthalpies of formation, of the studied sulphur heterocycles in the gaseous phase, were then derived. The results are interpreted in terms of structural contributions to the energetics of the substituted thiophenes, the internal consistency of the results is discussed and, whenever appropriate and possible, empirical correlations are suggested for the estimation of standard molar enthalpies of formation, at T=298.15 K, of substituted thiophenes. A Table of enthalpic increments for different group substituents in positions 2 or 3 of the thiophene ring has been established
M. A. V. Ribeiro da Silva, Ana Filipa L. O. M. Santos, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 2, 333Ð344
B2438 - Study of Energetics and Structure of 1,2,3-Benzotriazin-4(3H)-one and its 1H and Enol Tautomers
This paper reports an experimental and computational study on the energetics of 1,2,3-benzotriazin-4(3H) one. The standard (p = 0.1 MPa) molar enthalpy of formation of solid 1,2,3-benzotriazin-4(3H)-one, at T = 298.15 K, was derived from its standard massic energy of combustion measured by static bomb combustion calorimetry in oxygen. The Calvet high-temperature vacuum sublimation technique was used to measure the respective standard molar enthalpy of sublimation at T = 298.15 K. From these two experimentally determined thermodynamic parameters, we have calculated the standard molar enthalpy of formation of 1,2,3-benzotriazin-4(3H)-one in the gas phase at T = 298.15 K, (200.9 ( 3.8) kJ 3 mol 1. Interrelations between structure and energy for 1,2,3-benzotriazin-4(3H)-one, the tautomer 1,2,3-benzotriazin-4(1H)-one, and the enol tautomer 1,2,3-benzotriazin-4-ol were discussed based on density functional theory (DFT) calculations with the B3LYP hybrid functional and the 6-311??G(d,p) basis set. The gas-phase enthalpy of formation of 1,2,3-benzotriazin-4(3H)-one was estimated from quantum chemical calculations using the G3(MP2)//B3LYP composite method. Nucleus-independent chemical shifts (NICS) were also calculated with the purpose of analyzing the aromaticity of the benzenic and heterocyclic rings of the title molecule and others related tautomerically to it.
Margarida S. Miranda, M. Agostinha R. Matos, Victor M. F. Morais, Joel F. Liebman, J. Phys. Chem. B 2011, 115, 6616Ð6622
B2437 - Molecular energetics of alkyl substituted pyridine N-oxides. An experimental study
The standard (p¡ = 0.1 MPa) energies of combustion in oxygen, at T = 298.15 K, for the solid compounds 2-methylpyridine-N-oxide (2-MePyNO), 3-methylpyridine-N-oxide (3-MePyNO) and 3,5-dimethylpyridine-N-oxide (3,5-DMePyNO) were measured by static-bomb calorimetry, from which the respective standard molar enthalpies of formation in the condensed phase were derived. The standard molar enthalpies of sublimation, at the same temperature, were measured by Calvet microcalorimetry. From the standard molar enthalpy of formation in gaseous phase, the molar dissociation enthalpies of the NÐO bonds were derived, and compared with values of the dissociation enthalpies of other NÐO bonds available for other pyridine-N-oxide derivatives.
Joana I. T. A. Cabral, Ricardo A. R. Monteiro, Marisa A. A. Rocha, Luõs M. N. B. F. Santos, William E. Acree Jr., Maria D. M. C. Ribeiro da Silva, J Therm Anal Calorim (2010) 100:431Ð439
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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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