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B2436 - Thermochemical properties of three piperidine derivatives: 1-Benzyl-4-piperidinol, 4-benzylpiperidine and 4-piperidine-piperidine
The standard (po=0.1 MPa) molar energies of combustion for the crystalline 1-benzyl-4-piperidinol and 4-piperidine-piperidine, and for the liquid 4-benzylpiperidine, were measured by static bomb calorimetry, in oxygen, at T=298.15 K. The standard molar enthalpies of sublimation or vaporization, at T=298.15 K, of these three compounds were determined by Calvet microcalorimetry. Those values were used to derive the standard molar enthalpies of formation, at T=298.15 K, in their condensed and gaseous phase, respectively.
M. A. V. Ribeiro da Silva, Joana I. T. A. Cabral, Journal of Thermal Analysis and Calorimetry, Vol. 90 (2007) 3, 865Ð871
B2435 - Energetics and Structure of Nicotinic Acid (Niacin)
The standard molar enthalpies of formation and sublimation of crystalline (monoclinic, space group P21/c) nicotinic acid (NA), at 298.15 K, were determined as ?fHm¡(NA, cr))-344.7 ( 1.2 kJ á mol-1 and ?subHm¡(NA) ) 112.1 ( 0.5 kJ á mol-1 by using combustion calorimetry, drop-sublimation Calvet microcalorimetry, and the Knudsen effusion method. The experimental determinations were all based on a sample of NIST Standard Reference Material 2151, which was characterized in terms of chemical purity, phase purity, and morphology.
Elsa M. Goncalves, Carlos E. S. Bernardes, Hermõnio P. Diogo, Manuel E. Minas da Piedade
B2434 - Standard molar enthalpies of formation of some methylfuran derivatives
The standard (po = 0.1 MPa) molar enthalpies of formation ?fHo m (1), of the liquid 2-methylfuran, 5-methyl-2-acetylfuran and 5-methyl-2-furaldehyde were derived from the standard molar energies of combustion, in oxygen, at T = 298.15 K, measured by static bomb combustion calorimetry. The Calvet high temperature vacuum sublimation technique was used to measure the enthalpies of vaporization of the three compounds. The standard (po = 0.1 MPa) molar enthalpies of formation of the compounds, in the gaseous phase, at T = 298.15 K have been derived from the corresponding standard molar enthalpies of formation in the liquid phase and the standard molar enthalpies of vaporization. The results obtained were -(76.4 ± 1.2), -(253.9 ± 1.9), and -(196.8 ± 1.8) kJ mol-1, for 2-methylfuran, 5-methyl-2-acetylfuran, and 5-methyl2-furaldehyde, respectively.
Manuel A. V. Ribeiro da Silva, Luõsa M. P. F. Amaral, J Therm Anal Calorim (2010) 100:375Ð380
B2433 - Enthalpy increment and heat capacity of Pb3Bi
Enthalpy increments of Pb0.71Bi0.29 compound and enthalpy change associated with peritectic decomposition reaction of the compound were determined using high temperature Calvet calorimeter. The heat capacity of the compound was determined in the temperature range 230Ð440K using heat flow DSC. The enthalpy increment data was fitted into the following polynomial equations. ?T 298.15K (J/mol) = ?6492.2 + 21.2775T + 0.00919T2 ? 199, 341/T (298.15Ð457 K) The enthalpy of decomposition reaction of the compound at the peritectic temperature, 457 K, was found to be 984 J/mol. The heat capacity of the compound determined using DSC was fitted into the following polynomial equation. Cp (J/mol K) = 23.486 ? 0.01482T + 97, 338.4/T2 (228Ð457 K) The heat capacity values obtained from DSC were in reasonably good agreement with the values calculated from enthalpy increment equation and both were slightly higher than the heat capacity values calculated using NeumannÐKoppÕs rule.
Renu Agarwal, Pradeep Samui, Journal of Alloys and Compounds 508 (2010) 333Ð337
B2432 - Thermochemistry of chromone- and coumarin-3-carboxylic acid
The standard (p8 = 0.1 MPa) molar enthalpies of formation in the condensed state of chromone-3-carboxylic acid and coumarin-3-carboxylic acid were derived from the standard molar energies of combustion in oxygen at T = 298.15 K, measured by combustion calorimetry. The standard molar enthalpies of sublimation were obtained by Calvet microcalorimetry. From these values the standard molar enthalpies in the gaseous phase, at T = 298.15 K, were derived. Additionally estimates of the enthalpies of formation, of all the studied compounds in gas-phase, were performed using DFT and other more accurate correlated calculations (MCCM and G3MP2), together with appropriate isodesmic, homodesmic or atomization reactions. There is a reasonable agreement between computational and experimental results.
M. Agostinha R. Matos, Clara C. S. Sousa, Victor M. F. Morais, J Therm Anal Calorim (2010) 100:519Ð526
B2431 - Thermodynamic properties of strontium metaniobate SrNb2O6
The heat capacity and the enthalpy increments of strontium metaniobate SrNb2O6 were measured by the relaxation method (2Ð276 K), micro DSC calorimetry (260Ð320 K) and drop calorimetry (723Ð1472 K). Temperature dependence of the molar heat capacity in the form Cpm=(200.47±5.51)+(0.02937±0.0760)TÐ(3.4728±0.3115)?106/T 2 J KÐ1 molÐ1 (298Ð1500 K) was derived by the least-squares method from the experimental data. Furthermore, the standard molar entropy at 298.15 K Sm 0 (298.15 K)=173.88±0.39 J KÐ1 molÐ1 was evaluated from the low temperature heat capacity measurements. The standard enthalpy of formation ?fH0 (298.15 K)= Ð2826.78 kJ molÐ1 was derived from total energies obtained by full potential
J. Leitner, M. Hampl, K. Ruzicka, M. Straka, D. Sedmidubsk, P. Svoboda, Journal of Thermal Analysis and Calorimetry, Vol. 91 (2008) 3, 985Ð990
B2430 - The high temperature heat capacity of NpO2
LAPW electronic structure calculations within density functional theory.
O. Benes, P. Gotcu-Freis, F. Schwrer, R.J.M. Konings, Th. Fanghnel, J. Chem. Thermodynamics 43 (2011) 651Ð655
B2429 - Gaseous Phase Heat Capacity of Benzoic Acid
The gaseous phase heat capacity of benzoic acid (BA) was proven using the experimental technique called the Òin vacuum sublimation/vaporization Calvet microcalorimetry drop methodÓ. To overcome known experimental shortfalls, the gaseous phase heat capacity of BA monomer was estimated by abinitio calculations and compared with experimental results. Gaseous phase heat capacities of BA were directly derived via calculated harmonic frequencies obtained by density functional theory (DFT) (B3LYP, BLYP, BP86, with 6-311++G(d,p), TZVP, cc-pVTZ basis sets) and the second-order M¿ller-Plesset theory, MP2/6-311++G(d,p). To increase the accuracy of estimation of the thermal properties, a procedure based on the calculation of the heat capacity from quantum chemical calculations in combination with a heat capacity balance of isodesmic reactions is described and applied to calculate the gaseous phase heat capacity, Cp,m, of the monomeric species over the temperature range of (298.15 to 600) K. The gaseous phase thermodynamic properties of the monomeric form of the BA were also derived from the assignment of the fundamental vibrational frequencies using experimental IR spectra. An excellent agreement among the experimental gaseous phase heat capacities, the results obtained using the proposed ab initio procedure, and the results derived from the assignment of fundamental vibrational frequencies was found. The results for the monomeric form of the BA, directly or indirectly obtained, and conclusions of this work strongly support the thesis that the gaseous phase heat capacity data as currently found in the literature are underestimated to the order of 20 %.
Luõs M. N. B. F. Santos, Marisa A. A. Rocha, Lõgia R. Gomes, Bernd Schrder, Joao A. P. Coutinho, J. Chem. Eng. Data 2010, 55, 2799Ð2808
B2428 - Excess enthalpies of ternary mixture consisting of tert-butyl methyl ether, ethanol and heptane
Excess molar enthalpies, measured at 298.15 K in a Calvet microcalorimeter, are reported for {x1tert-butyl methyl ether (MTBE)+x2ethanol (EtOH)+(1Ðx1Ðx2)heptane}. Smooth representations of the results are presented and used to construct constant excess molar enthalpy contours on Roozeboom diagrams.
M. M. Mato, P. V. Verdes, M. Illobre, J. L. Legido, M. I. Paz Andrade, Journal of Thermal Analysis and Calorimetry, Vol. 92 (2008) 1, 185Ð189
B2427 - The effect of solid-liquid effluents from anaerobic digesters on soil microbial activity. A calorimetric study
A calorimetric procedure is developed to study the effect on the soil of the effluents resulting for the anaerobic digestion of slaughtering houses residues. DSC was used to study the pyrolysis properties of the effluent and the soil while isothermal calorimetry is applied to study the microbial activity in the effluent and to assess on its effect on the microbial activity of the soil where the industrial digester will be situated. The calorimetric data were studied together with the chemical and biological properties of that residue. Results showed that effluent is constituted by low levels of carbon and high levels of nitrogen. The powerÐtime curves of the effluent have the typical shape of microbial growth yielding microbial growth rate constants between 0.37 and 0.53 hÐ1 for about 4 and 11 h. The addition of the effluent to the soil decreases the heat of pyrolysis with time and stimulates the heat flow rate of the microbial metabolism.
N. Barros, B. Ramajo, J. R. Garc'a, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 3, 831Ð835
B2426 - Equilibrium desorption isotherms of water, ethanol, ethyl acetate, and toluene on a sodium smectite clay
Desorption isotherms for water, ethanol, ethyl acetate and toluene from a sodium smectite clay have been determined by both dynamic vapor sorption (DVS) measurements and Knudsen thermogravimetry (KTGA), at the exception of toluene that was measured only by the DVS method. The results obtained using these two methods were in satisfactory agreement, providing reliable insight into the desorption process, with certain lack of precision for ethyl acetate. The observed desorption behaviour suggests a liquid like phase at high volatile load, and a sorbed state in which molecules interact with the counter ions, at low volatile contents. However, the isotherms for water determined at various temperatures nearly superposed when plotted as a function of water activity, indicating the strength of the interactions in the clayÐwater system to remain of the same order of magnitude as that in bulk water, consistent with previous ab initio calculations.
Pascal Clausen, Marco Signorelli, Andreas Schreiber,,Eric Hughes, Christopher J. G. Plummer, Dimitrios Fessas, Alberto Schiraldi, Jan-Anders E. Manson, J Therm Anal Calorim (2009) 98:833Ð841
B2425 - Molar Heat Capacities of Some Derivatives of Uridine and 2?-Deoxyuridine
The molar heat capacities Cp,m of seven crystalline compounds (uridine, 2?-deoxyuridine, 5-iodouridine, 5-bromouridine, 5-iodo-2?-deoxyuridine, 5-bromo-2?-deoxyuridine, and 5-methyl-2?-deoxyuridine (thymidine)) were determined using a differential scanning calorimeter (SETARAM TG-DSC 111). The measurements were made over the temperature range from (298.15 to 368.15) K. The values of molar heat capacities versus temperature Cp,m ) f(T) were determined. The standard molar heat capacities Cp,m 0 were compared with those calculated by the Chickos method. The contributions of the C-CH3 group, as well as Br and I atoms, in the value of Cp,m 0 were evaluated.
Piotr Szterner, J. Chem. Eng. Data 2008, 53, 1892Ð1896
B2424 - Fireproofing of polyurethane by organophosphonates. Study of degradation by simultaneously TG/DSC
In this work, we have studied the degradation processes of polyurethane containing phosphonate groups used as a fireproofing agent. These studies are undertaken by simultaneous thermogravimetry (TG) and differential scanning calorimetry (DSC) measurements. It is found that fireproofing agents with phosphonate react with oxygen in the air and prevent the complete combustion of the material. It is also found that the energy released during combustion is low when comparison is performed with other fireproofing materials.
B. Youssef, B. Mortaigne, M. Soulard, J. M. Saiter, Journal of Thermal Analysis and Calorimetry, Vol. 90 (2007) 2, 489Ð494
B2423 - Adsorption of CO2 on Hydrotalcite-Derived Mixed Oxides: Sorption Mechanisms and Consequences for Adsorption Irreversibility
Magnesium-aluminum double oxides derived from the thermal treatment of layered hydroxides (hydrotalcites) have been tested for CO2 adsorption. The effects of various preparation parameters, such as the incorporated cation (K or Na), the mode of addition of magnesium and aluminum precursors, the presence of sonication, and the calcination temperature, on the adsorption capacity under mild conditions were studied using thermogravimetry and calorimetry. Calorimetric and FTIR data were used to explain the adsorption mechanisms leading to the undesirable irreversible adsorption. This adsorption was related to the formation of unidentate CO2-adsorbent species with the strongest adsorption sites, whereas bidentate and surface bicarbonates lead to highly reversible adsorption. In conclusion, preparation procedures that lead to an increase in the strength of basic sites do not lead to significant increases in the adsorption capacity, but rather lead to more difficult regeneration of the saturated support.
Marta Leon, Eva Dõaz, Simona Bennici, Aurelio Vega, Salvador Ordonez, Aline Auroux, Ind. Eng. Chem. Res. 2010, 49, 3663Ð3671
B2422 - Influence of the metal oxide support on the surface and catalytic properties of sulfated vanadia catalysts for selective oxidation of methanol
The selective oxidation of methanol to dimethoxymethane (DMM) was performed over a series of binary vanadia-based oxides (V2O5-TiO2, V2O5-ZrO2, V2O5-Al2O3 and V2O5-CeO2) and the corresponding sulfated catalysts. The physicochemical properties of catalysts were characterized by BET, Raman, XPS, TPRÐMS, ammonia adsorption calorimetry and sulfate TPDÐMS techniques. The strength of the sulfate-support interaction depends on the nature of the oxide support and increases in the following order CeO2 > Al2O3 > ZrO2 > TiO2. The catalytic reactivity was correlated with the nature of VAO-support bonds. Sample V2O5-TiO2 exhibits the highest intrinsic activity of methanol oxidation. With the addition of sulfate, the selectivity to DMM was enhanced whereas the turnover frequency (TOF) value of vanadium sites decreased, with a rate depending on the strength of sulfate-support bonds. The best catalyst (V2O5-TiO2-SO42-) with higher DMM yield presented higher reducibility, proper acidity and moderate strength of sulfate species.
Hongying Zhao, Simona Bennici, Jingxuan Cai, Jianyi Shen, Aline Auroux, Journal of Catalysis 274 (2010) 259Ð272
B2421 - Activated carbon porosity tailoring by cyclic sorption / decomposition of molecular oxygen
Activated-carbon pore size tailoring is usually achieved by pore size reduction, pore size widening or more rarely by direct activation. Successive widening cycles composed of an initial molecular oxygen sorption step, followed by a carbonization step under nitrogen, have been applied to three different materials in order to study their gradual pore size modifications. For years, the whole microporosity obtained after several cycles is known to present better pore size distribution than those inherited from conventional activations. Moreover, as shown in the present paper, the gradual obtained microporosities cover a wide and valuable range of porous textures highly dependent on the initial material origin and initial activation. Gradual mean pore size evolutions of 1 or 2 A¡ per cycle were observed linked to a simultaneous increase in microporous specific volume in the case of pitch-based and coconut activated carbons, respectively. Comparatively, the microporous specific volume of a commercial coconut carbon molecular sieve was increased by 26% without modification of its mean pore size and therefore of its sieving effect. Those results have been used to test a simple textural model of activated carbon porosity proposed in the recent literature.
X. Py, A. Guillot, B. Cagnon, Carbon 41 (2003) 1533Ð1543
B2420 - Contributions of hemicellulose, cellulose and lignin to the mass and the porous properties of chars and steam activated carbons from various lignocellulosic precursors
In this study, contributions of hemicellulose, cellulose and lignin to the mass and the porous properties of chars and activated carbons from various lignocellulosic materials were studied. A predictive calculation was established using the experimental results obtained for the three components separately to evaluate the carbonization and activation yields and their respective contributions to the chars and to the subsequent activated carbons of various precursors in term of weight fraction. These equations were validated. The results showed that lignin can be considering as being the major contributor of all chars and activated carbons. Besides, the evolution of the mean pore size versus the specific porous volume showed that each component contributes to the porosity of chars and activated carbons whatever is its weight contribution.
Beno"t Cagnon, Xavier Py, Andr Guillot, Fritz Stoeckli, Grard Chambat, Bioresource Technology 100 (2009) 292Ð298
B2419 - Thermodynamic properties of liquid silverÐgallium alloys determined from e.m.f. and calorimetric measurements
The thermodynamic properties of the liquid AgÐGa alloys were determined using e.m.f. and calorimetric methods. In the e.m.f. method, solid oxide galvanic cells were used with zirconia electrolyte. The cells of the type W, AgxGa(1-x), Ga2O3 // ZrO2 + (Y2O3)//FeO, Fe, W were used in the temperature range from 1098 K to 1273 K, and in the range of mole fraction from xGa = 0.1 to xGa = 1.0. At first, the Gibbs free energy of formation of pure solid gallium oxide, Ga2O3, from pure elements was derived. Using values of the measured e.m.f. for the cell with xGa = 1.0, the following temperature dependence was obtained: ?fGm(Ga2O3) (± 4 kJ.mol 1) = -1061.7235 + 0:2899T/K: Next, the activity of the gallium was derived as a function of the alloy composition from the values of the measured e.m.f. Activities of silver were calculated using the GibbsÐDuhem equation. The drop calorimetric measurements were carried out at two temperatures, viz. 923 K and 1123 K, using a Setaram MHTC calorimeter. Integral enthalpies of mixing of liquid binary alloys were determined at those temperatures. Finally, thermodynamic properties of the liquid alloys were described with the RedlichÐKister equation using ThermoCalc software
Dominika Jendrzejczyk-Handzlik, Krzysztof Fitzner, J. Chem. Thermodynamics 43 (2011) 392Ð398
B2418 - Enthalpy of formation of selected mixed oxides in a CaOÐSrOÐBi2O3ÐNb2O5 system
The heats of drop-solution in 3Na2O+4MoO3 melt at 973K and 1073K for calcium and strontium carbonates, Bi2O3, Nb2O5 and several stoichiometric mixed oxides in CaOÐNb2O5, SrOÐNb2O5 and Bi2O3ÐNb2O5 systems were measured using a Setaram Multi HTC-96 calorimeter. The values of enthalpy of formation from constituent binary oxides at 298 K, ?oxH, were derived for the mixed oxides under investigation: ?oxH(CaNb2O6) =?132.0±23.8 kJ mol?1, ?oxH(Ca2Nb2O7) =?208.0±31.9 kJ mol?1, ?oxH(SrNb2O6) =?167.9±19.1 kJ mol?1, ?oxH(Sr2Nb2O7) =?289.2±37.5 kJ mol?1 and ?oxH(BiNbO4) =?41.9±11.1 kJ mol?1. Additionally, the values ?oxH for other mixed oxides with different stoichiometries were estimated on the basis of these experimental results.
J. Leitner, M. Nevriva, D. Sedmidubsky, P. Vonka, Journal of Alloys and Compounds 509 (2011) 4940Ð4943
B2417 - Solubility diagrams in solventÐantisolvent systems by titration calorimetry. Application to some pharmaceutical compounds in waterÐethanol mixtures
Isothermal titration calorimetry (ITC) has been used to develop a method to construct the solid-liquid equilibrium line in ternary systems containing the solute to precipitate and an aqueous mixed solvent. The method consists in measuring the heat of dissolution of a solid component (the solute) during successive additions of the liquid solvent. The cumulated heat, resulting from the successive heat peaks obtained for the different injections of known volumes of solvent, plotted vs. the ratio of the numbers of moles nsolvent/nsolute is represented by two nearly straight lines. The intercept of the two lines gives the solubility limit and the corresponding enthalpy of dissolution of the solute in the solvent. Solubility diagrams have been established at 303.15 K in binary mixed solvents ethanolÐwater over the whole concentration range for seven compounds of pharmaceutical interest, namely: urea, phenylurea, l-valine, dl-valine, l-valine ethyl ester hydrochloride, tris(hydroxymethyl)amino methane.
M. H. Hamedi, J.-P. E. Grolier, Journal of Thermal Analysis and Calorimetry, Vol. 89 (2007) 1, 87Ð92
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