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B2556 - Studies of homogeneous interactions of N-acetyl-N?-methyl-l-?-amino acid amides in water at 298.15 K
The enthalpies of dilution of aqueous solutions of N-acetyl-N?-methyl-l-glycinamide (AcGlyNHCH3), N-acetyl-N?-methyl-l-?-alaninamide (AcAlaNHCH3), N-acetyl-N?-methyl-l-?-valinamide (AcValNHCH3), N-acetyl-N?-methyl-l-?-leucinamide (AcLeuNHCH3) (BACHEM) and N-acetyl-N?-methyl-l-?-serinamide (AcSerNHCH3), N-acetyl-N?-methyl-l-?-threoninamide (AcThrNHCH3), in water at 298.15 K have been measured. These data were used to calculate the homogeneous enthalpic pair interaction coefficients based on McMillanÐMayer's theory.
Bart?omiej Pa?ecz, Sylwia Belica, Henryk Piekarski, Andrzej J--?wia, Thermochimica Acta, 489 (2009) 1-4
B2555 - Freezing in non-acclimated oats. II: Thermal response and histology of recovery in gradual and rapidly frozen plants
Freezing in winter cereals is a complex phenomenon that can affect various plant tissues differently. To better understand how freezing affects specific tissue in the over wintering organ (crown) of winter cereal crops, non-acclimated oats (Avena sativa L.) were gradually frozen to ?3 ¡C and tissue damage during recovery was compared to plants that had been supercooled to ?3 ¡C and then frozen suddenly. Percentage of total water frozen, was the same whether crowns were frozen suddenly or gradually although the rate of freezing was considerably different. For example, all available water froze within 3 h in suddenly frozen crowns but it took more than 15 h for all available water to freeze in gradually frozen crowns. When plants were suddenly frozen, cells in the apical meristem were disrupted and apparently killed. In these plants re-growth was limited or non-existent. In contrast, the apical region of plants that were slowly frozen appeared undamaged but extensive vessel plugging was observed in cells of the lower crown, possibly from accumulation of phenolics or from microbial proliferation. These histological observations along with the calorimetric analysis suggested that the apical region was killed by intracellular freezing when frozen suddenly while the crown core was damaged by a process, which either induced production of putative phenolic compounds by the plant and/or permitted what appeared to be microbial proliferation in metaxylem vessels
David P. Livingston III, Shyamalrau P. Tallury, Thermochimica Acta, 481 (2009) 20-27
B2554 - Thermodynamics of Ketone + Amine Mixtures. Part VIII. Molar Excess Enthalpies at 298.15 K for n-Alkanone + Aniline or + N-Methylaniline Systems
Molar excess enthalpies, HmE , at 298.15 K and atmospheric pressure have been determined over the entire mole fraction range, using a Tian-Calvet microcalorimeter, for the systems: propanone, 2-butanone, 2-pentanone, or 2-heptanone + aniline or + N-methylaniline. The negative HmE values obtained for all of the mixtures reveal that interactions between unlike molecules are prevalent. Aniline solutions show more negative HmE values due to stronger amine-ketone interactions compared to those in N-methylaniline solutions. In addition, HmE increases with the size of the alkanone, which may be interpreted in terms of a weakening of interactions between unlike molecules. HmE varies somewhat differently in N-methylaniline solutions, probably due to the positive contribution to HmE is here more important. Molar excess internal energies at constant volume, UVmE, have been determined from the present HmE data using our previous measurements on molar excess volumes, compressibilities, and isothermal expansion coefficients. UVmE behaves similarly toHmE.UVmE values are much higher than those of HmE, which remarks the importance of the contribution of the equation of state term to HmE .
Ivan Alonso, Ismael Mozo, Isa'as Garc'a de la Fuente, Juan Antonio Gonz alez, Jose Carlos Cobos
B2553 - Relationship between adsorption properties of PtÐCu/SiO2 catalysts and their catalytic performance for selective hydrodechlorination of 1,2-dichloroethane to ethylene
Microcalorimetric adsorption technique was employed to study the interaction of the reactants and product in the 1,2-dichloroethane hydrodechlorination over Pt/SiO2, Cu/SiO2 and PtÐCu/SiO2 catalysts in order to understand the high selectivity towards C2H4 on the Pt/SiO2 catalyst modified by Cu. When the adsorption properties of the reactants and product on bimetallic catalysts were compared with those on monometallic counterparts, significant differences in the strength and number of adsorption sites concerning the reactants and product were evidenced. The adsorption properties of the bimetallic catalysts could be attributed to the change in Pt surface structure modified by Cu, studied by the microcalorimetry and FTIR of CO adsorption. Relating the adsorption properties with high ethylene selectivity on bimetallic catalysts, we inferred that high ethylene selectivity on bimetallic catalysts could be attributed to the moderate adsorption and activation of reactants and product. This work gave the direct evidence of high C2H4 selectivity in 1,2-dichloroethane hydrodechlorination reaction on the PtÐCu/SiO2 catalysts from the energetic point of view.
Lin Li, Xiaodong Wang, Aiqin Wang, Jianyi Shen, Tao Zhang, Thermochimica Acta, 494 (2009) 99-103
B2552 - Hydration of ?-chymotrypsin: Excess partial enthalpies of water and enzyme
A novel method has been developed for studying simultaneously the excess partial enthalpies of water and the enzyme in the entire range of water content. Bovine pancreatic ?-chymotrypsin was used as a model enzyme. The proposed method includes the measurements of the enthalpies of solution of the dried and hydrated enzyme in water at 25 ¡C. From these thermochemical data the excess partial enthalpies of water and ?-chymotrypsin were calculated. The partial quantities are very sensitive to the changes in the state of water and ?-chymotrypsin. A transition from the glassy to the flexible state of ?-chymotrypsin is accompanied by significant changes in the excess partial enthalpies of water and ?-chymotrypsin. This transition appears at water weight fraction (w1) of 0.06 when charged groups of ?-chymotrypsin are covered. Excess partial quantities reach their fully hydrated values at w1 > 0.4 when coverage of both polar and weakly interacting surface elements is complete.
Vladimir A. Sirotkin , Aigul V. Khadiullina, Thermochimica Acta, 522 (2011) 205-210
B2551 - Thermodynamic investigation of several natural polyols (II). Heat capacities and thermodynamic properties of sorbitol
The low-temperature heat capacity Cp,m of sorbitol was precisely measured in the temperature range from 80 to 390 K by means of a small sample automated adiabatic calorimeter. A solidÐliquid phase transition was found at T=369.157 K from the experimental CpÐT curve. 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 355 K, Cp,m/J KÐ1 molÐ1=170.17+157.75x+128.03x2Ð146.44x3Ð335.66x4+177.71x5 +306.15x6, x= [(T/K)Ð217.5]/137.5. In the temperature range of 375 to 390 K, Cp,m/J KÐ1 molÐ1=518.13+3.2819x, x=[(T/K)Ð382.5]/7.5. The molar enthalpy and entropy of this transition were determined to be 30.35 0.15 kJ molÐ1 and 82.22 0.41 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 390 K with an interval of 5 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, Q. Shi, Y. S. Li, S. X. Wang, Journal of Thermal Analysis and Calorimetry, Vol. 91 (2008) 2, 463Ð469
B2550 - Polyaniline/1-tetradecanol composites. Form-stable PCMS and electrical conductive materials
Polyaniline (PANI)/1-tetradecanol (TD) composite materials, a kind of novel composite that can conduct electricity and store thermal energy at the same time, thus possess the ability to endure certain heat shock, were prepared for the first time. FTIR and XRD results showed that there were some interactions existed between PANI and TD. The thermal stability of the composites exhibited both the characteristics of PANI and TD. The DSC experiments showed that the highest phase change enthalpy of the composites could be as 73% as that of TD, indicating it was a good form-stable phase change material. The thermal conductivity of the composites was also improved. The AC (Alternating Current) conductivity of the composites was enhanced to close to that of PANI when the mass fraction of PANI in the composite was increased to 46%. Heat shock experiments showed that the heat shock resistibility of the composite was greatly improved comparing to that of pure PANI.
J. L. Zeng, J. Zhang, Y. Y. Liu, Z. X. Cao, Z. H. Zhang, F. Xu, L. X. Sun, Journal of Thermal Analysis and Calorimetry, Vol. 91 (2008) 2, 455Ð461
B2549 - Thermal conductivity enhancement of MWNTS on the PANI/tetradecanol form-stable PCM
We prepared PANI/tetradecanol/MWNTs composites via in-situ polymerization. DSC results indicated that the composites are good form-stable phase change materials (PCMs) with large phase change enthalpy of 115 J gÐ1. The MWNTs were randomly dispersed in the composites and significantly enhanced the thermal conductivity of the PCMs from 0.33 to 0.43 W mÐ1 KÐ1. The form-stable PCMs wonÕt liquefy even it is heated at 80¡C, so that the MWNTs were fixed in the composite and the phase separation of the MWNTs from PANI/tetradecanol/MWNTs composites wonÕt occur.
J. L. Zeng, Y. Y. Liu, Z. X. Cao, J. Zhang, Z. H. Zhang, L. X. Sun, F. Xu, Journal of Thermal Analysis and Calorimetry, Vol. 91 (2008) 2, 443Ð446
B2548 - Phase transformation and phase diagram at equilibrium in the CuÐNiÐSn system
The CuÐNiÐSn ternary phase diagram in the Cu rich side has not been experimentally determined or calculated at low temperatures. Two Cu9NixSn alloys with x=2 and 6 mass% Sn were studied. The precipitation sequence during the ageing and phases responsible for the strengthening were determined.
F. Sadi, C. Servant, Journal of Thermal Analysis and Calorimetry, Vol. 90 (2007) 2, 319Ð323
B2547 - Study on the effect of mechanical alloying on properties of ZnÐSb alloy
The effect of mechanical alloying on ZnÐSb alloy system is investigated with X-ray diffraction (XRD), laser grain size analysis and differential scanning calorimetry (DSC) respectively. The results of laser particle size analysis shows that the particle size decreases with increasing of the grinding time between 0 and 24 h. XRD and DSC results indicate that longer the grinding time of ZnÐSb is, the more content of Zn4Sb3 become in the product in this process.
Z. L. Xiao, D. Liu, C. F. Wang, Z. Cao, X. F. Zhan, Z. L. Yin, Q. Y. Chen, H. L. Liu, F. Xu, L. X. Sun, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 2, 513Ð515
B2546 - Phase diagram and electrical conductivity of the CeBr3ÐCsBr binary system
Phase equilibrium in the CeBr3ÐCsBr binary system was established from differential scanning calorimetry (DSC). This system includes three compounds, namely Cs3CeBr6, Cs2CeBr5 and CsCe2Br7; and three eutectics located at CeBr3 molar fraction x = 0.125; 0.459 and 0.700, respectively. Cs3CeBr6 undergoes a solidÐsolid phase transition at 712 K and melts congruently at 1034 K. Cs2CeBr5 decomposes in the solid state into Cs3CeBr6 and CsCe2Br7 at 685 K. The third compound, CsCe2Br7, melts congruently at 877 K. The electrical conductivity of CeBr3ÐCsBr liquid mixtures was measured down to temperatures below solidification over the whole composition range. Results obtained are discussed in term of possible complex formation.
Leszek Rycerz, Ewa Ingier-Stocka, Marcelle Gaune-Escard, J Therm Anal Calorim (2009) 97,1015Ð1021
B2545 - Influence of chemical structure on critical parameters for dimethyl carbonate+alkane systems
In order to study the dependence of non-universal critical quantities on the molecular structure, heat capacities per unit volume for the dimethyl carbonate+(heptane, octane, nonane, decane or tridecane) critical mixtures near their upper consolute point are measured. The data are obtained at atmospheric pressure as a function of temperature in the homogeneous and heterogeneous regions by means of a differential scanning calorimeter. The exponent and amplitudes that characterises the observed critical anomaly are determined from experimental data, being their values coherent to previous results; in addition, the critical amplitudes of the correlation length was calculated from critical amplitudes using the universality of the two-scale factor. The influence of the alkane length on the critical temperature and heat capacity critical amplitude are analysed.
M. Souto-Caride, J. Troncoso, J. Peleteiro, E. Carballo, L. Romani, Journal of Thermal Analysis and Calorimetry, Vol. 89 (2007) 1, 25Ð29
B2544 - Use of isothermal microcalorimetry for prediction of oxidative stability of several amino acids
Isothermal microcalorimetry has been applied as a method for predicting (in)stability of ascorbic acid and several amino acids that undergo oxidative degradation in aqueous media. The fast and simple method involved the addition of different amounts of hydrogen peroxide. The appearance of the heat flow curves gave a clear general indication of how stability was influenced. The accuracy of the microcalorimetric result was investigated by comparing it with an HPLC assay and a good agreement between the results of both methods was demonstrated. It was also established that susceptibility to oxidative degradation decreases in the following order: cysteine, methionine, ascorbic acid, tyrosine and tryptophan
R. Roskar, M. Vivoda, V. Kmetec, Journal of Thermal Analysis and Calorimetry, Vol. 92 (2008) 3, 791Ð794
B2543 - Thermodynamics of azurin folding. The role of copper ion
The role played by the metal ion in thermodynamics of azurin folding was addressed by studying the thermal denaturation of the apo-form by differential scanning calorimetry (DSC), and by comparing the results with data concerning the holo protein. The thermal unfolding experiments showed that at 25¡C the presence of metal ion increases the thermodynamic stability of azurin by 24 kJ molÐ1. A comparison between the unfolding and the copper binding free energies allow us to assert that the unfolded polypeptide chain binds copper and subsequently folds into native holo azurin, being this the thermodynamically most favourable process in driving azurin folding.
M. Pappalardo, M. F. M. Sciacca, D. Milardi, D. M. Grasso, C. La Rosa, Journal of Thermal Analysis and Calorimetry, Vol. 93 (2008) 2, 575Ð581
B2542 - Heat Capacities of Tetracene and Pentacene
New solid state heat capacity data for tetracene and pentacene are reported in the temperature range (258 to 600) K. The heat capacity measurements were performed using the step method with a Setaram MicroDSC III calorimeter (Institute of Chemical Technology, Prague) and a Setaram TG-DSC 111 (University of Alberta) calorimeter. These new heat capacity data are shown to be in good agreement with one another and with several solid state constant-pressure heat capacity estimation methods and quantum mechanical calculations. The new results highlight errors in the solid state heat capacity and melting point databases for polynuclear aromatic hydrocarbons.
Michal Fulem, Vaclav Lastovka, Martin Straka, Kvetoslav Ruzicka, John M. Shaw
B2541 - Aggregation in aqueous media of tri-block copolymers tuned by the molecular selectivity of cyclodextrins
The water cyclodextrin poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) mixtures have been investigated to explore the temperature effect on the aggregation of the copolymer in the presence of cyclodextrins (CDs). The CDs with different cavity sizes were chosen because they may include either the hydrophilic poly(ethylene oxides) block or both kinds of blocks. The differential scanning calorimetry and viscosity experiments straightforwardly evidenced that the critical micellar temperature is shifted to larger values by adding a CD which is able to include the middle poly(propylene oxide) block while it is not influenced by the presence of CD which is selective to the poly(ethylene oxide) block. The enthalpy of aggregation decreases upon the CD addition for all the investigated systems.
Rosario De Lisi, Giuseppe Lazzara, J Therm Anal Calorim (2009) 97, 797Ð803
B2540 - Heat Capacities of Some Liquid ?,?-Alkanediols within the Temperature Range between (293.15 and 353.15) K
The heat capacities at constant pressure of 1,2-ethanediol (1,2-EtD), 1,3-propanediol (1,3-PrD), 1,4-butanediol (1,4-BuD), 1,5-pentanediol (1,5-PeD), and 1,7-heptanediol (1,7-HpD) were measured within the temperature range from (293.15 to 353.15) K. The heat capacities of three other compounds, 1,6-hexanediol (1,6-HxD), 1,8-octanediol (1,8-OcD), and 1,9-nonanediol (1,9-NoD), were also measured between their melting point and 353.15 K. All measurements were performed by means of a DSC III (Setaram) differential scanning calorimeter. Assuming that the molar heat capacity shows an additive character, a simple equation was proposed that allows one to describe Cp values of liquid ?,?-alkanediols as a function of temperature and the alkyl chain length with an accuracy below 1 %.
Pawe? Goralski, Mariola Tkaczyk, J. Chem. Eng. Data 2008, 53, 1932Ð1934
B2539 - Thermophysical Characterization of Liquids Using Precise Density and Isobaric Heat Capacity Measurements As a Function of Pressure
compressibility, and isobaric and isochoric heat capacity of liquids as a function of temperature and pressure is analyzed in detail. The procedure is based on the experimental determination of both the density using the Anton Paar DMA512P vibrating tube densimeter and the isobaric heat capacity using the micro DSCII calorimeter from Setaram, which was recently adapted to operate up to 70 MPa. All properties are derived from these measurements using appropriate thermodynamic relations. To estimate the attained accuracy, densities for hexane, nonane, decane, undecane, dodecane, tridecane, tetradecane, 1-hexanol, and toluene were measured in the temperature interval of (283.15 to 323.15) K and at selected pressures between (0.1 and 60) MPa. Isobaric heat capacities for the same liquids (except toluene) were previously reported.9 The comparison between the complete set of properties for these liquids and selected literature data shows that this methodology allows us to get an accurate description of the thermodynamic behavior of liquids as a function of temperature and pressure.
Jose Luis Valencia, Diego Gonzalez-Salgado, Jacobo Troncoso, Jose Peleteiro, Enrique Carballo, Luis Romanõ, J. Chem. Eng. Data 2009, 54, 904Ð915
B2538 - Heat Capacities of Some Liquid ?,?-Alkanediamines in the Temperature Range between (293.15 and 353.15) K
Heat capacities at constant pressure of 1,2-diaminoethane (1,2-DAEt) and 1,3-diaminopropane (1,3-DAPr) were measured within the temperature range from (293.15 to 353.15) K. The heat capacities of four other compounds, 1,4-diaminobutane (1,4-DABu), 1,6-diaminohexane (1,6-DAHx), 1,7-diaminoheptane (1,7-DAHp), and 1,9-diaminononane (1,9-DANo), were also measured between their melting point and 353.15 K. All measurements were performed by means of a DSC III (Setaram) differential scanning calorimeter. Assuming that molar heat capacity shows an additive character, a simple equation was proposed that allows one to describe Cp values of liquid ?,?-alkanediamines as a function of temperature and the alkyl chain length with an accuracy below 0.5 %.
Pawe? Goralski, Mariola Tkaczyk, J. Chem. Eng. Data 2010, 55, 953Ð955
B2537 - Thermodynamic and Acoustic Properties of Mixtures of 1,6-Dichlorohexane with Heptane from (293 to 313) K
For {xCl(CH2)6Cl + (1 - x) n-C7H16}, densities F were measured with a vibrating-tube densimeter at (293.15, 298.15, 303.15, 308.15, and 313.15) K, covering the whole composition range. From the densities the corresponding isobaric expansivities Rp and the excess molar volumes VE were calculated. At the same temperatures, the molar heat capacities at constant pressure Cp were also measured over the whole composition range using a differential scanning calorimeter (DSC III from Setaram), and excess molar heat capacities at constant pressure Cp E were calculated therefrom. In addition, ultrasound speeds u were determined with a pulse-echo-overlap apparatus. From these results, isentropic compressibilities ?S, isothermal compressibilities ?T, molar heat capacities at constant volume CV, and internal pressures ? were obtained for this system at all five temperatures. The VE are negative throughout; they are somewhat skewed with minima around x ) 0.6, and they become less negative with decreasing temperature. The Cp E are all negative and strongly asymmetric with minima around x ) 0.3 and rather broad shoulders at larger mole fractions of 1,6-dichlorohexane. With decreasing temperature, the Cp E(x) curves become less negative with more pronounced shoulders, which behavior is reminiscent of the onset of a W-shaped composition dependence.
Miros?aw Chorazewski, Pawe? Goralski, Ma?gorzata Hrynko, Jean-Pierre Grolier, Emmerich Wilhelm, J. Chem. Eng. Data 2010, 55, 5471Ð5477
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