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B2536 - Heat capacity, enthalpy and entropy of calcium niobates
Heat capacity and enthalpy increments of calcium niobates CaNb2O6 and Ca2Nb2O7 were measured by the relaxation time method (2Ð300 K), DSC (260Ð360 K) and drop calorimetry (669Ð1421 K). Temperature dependencies of the molar heat capacity in the form Cpm=200.4+0.03432TÐ3.450á106/T 2 J KÐ1 molÐ1 for CaNb2O6 and Cpm=257.2+0.03621TÐ4.435á106/T 2 J KÐ1 molÐ1 for Ca2Nb2O7 were derived by the least-squares method from the experimental data. The molar entropies at 298.15 K, Sm0(CaNb2O6, 298.15 K)=167.3±0.9 J KÐ1 molÐ1 and Sm0 (Ca2Nb2O7, 298.15 K)=212.4±1.2 J KÐ1 molÐ1, were evaluated from the low temperature heat capacity measurements. Standard enthalpies of formation at 298.15 K were derived using published values of Gibbs energy of formation and presented heat capacity and entropy data: ?fH0(CaNb2O6, 298.15 K)= Ð2664.52 kJ molÐ1 and ?fH0(Ca2Nb2O7, 298.15 K)= Ð3346.91 kJ molÐ1.
J. Leitner, K. Ruzicka, D. Sedmidubsk, P. Svoboda, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 2, 397Ð402
B2535 - Heterogeneous soft acid catalysis of the sucrose hydrolysis
Using a micro-calorimetrical DSC we have compared the acid-catalyzed inversion of sucrose in homogeneous and heterogeneous systems. Acetic acid was chosen as catalyst for homogeneous system, and several carboxylic cationites were used as heterogeneous catalysts. The kinetic apparent parameters (A, E, kap) for all the systems were calculated from DSC data with FriedmannÕs method and catalytic constant, kcat 323, was further inferred. We found that the specific catalyst efficiency, qcat, in heterogeneous system is over 5000 times higher than in case of homogeneous ones. The activity of heterogeneous carboxylic systems is still about 30 times larger than those of a strong mineral acid in homogeneous catalysis. The results indicate the high efficiency of heterogeneous systems for soft acid catalysis of the sucrose hydrolysis
Dorina Chambre, Maria-Raluca Szabo, C. Popescu, Cornelia Idi*oiu, Journal of Thermal Analysis and Calorimetry, Vol. 94 (2008) 2, 417Ð420
B2534 - Recommended vapor pressures for thiophene, sulfolane, and dimethyl sulfoxide
Recommended vapor pressure data for important industrial solvents, thiophene (CAS RN: 110-02-1), sulfolane (CAS RN: 126-33-0), and dimethyl sulfoxide (CAS RN: 67-68-5), were developed by the simultaneous correlation of vapor pressure and related thermal data (heat capacities of condensed phases, ideal gas heat capacities and calorimetrically determined enthalpies of vaporization). For sulfolane and dimethyl sulfoxide, new vapor pressure data were obtained using the static method in the temperature interval from 273 to 308 K. Liquid heat capacities and calorimetric enthalpies of vaporization were taken from the literature and/or determined by Calvet calorimetry. The thermodynamic properties in the ideal gaseous state were calculated using the methods of statistical thermodynamics based on experimental as well as calculated fundamental vibrational frequencies and molecular structure data. Comparisons with literature values are shown for all measured and derived properties.
Michal Fulem, Kvetoslav Rzicka, Martin Rzicka, Fluid Phase Equilibria 303 (2011) 205Ð216
B2533 - Calorimetric and EPR studies of the thermotropic phase behavior of phospholipid membranes
Transmission electron micrographs (TEM) showed that liposome vesicles prepared from DL-a-phosphatidylcholine dimyristoyl (1,2-ditetradecanoyl-rac-glycerol-3-phosphocholine) (DMPC) by the modified reverse-phase evaporation method (mREV) were spherical in shape and in majority of them were less than 100 nm in diameter. Differential scanning calorimetry (DSC) method was used to determine the influence of cholesterol content and pH of Tris-HCl buffer used for the preparation of liposomes on the temperature of phase transition TC of phospholipids which form the investigated liposome vesicles. The use of DSC method made it possible to determine not only the temperature of the main phase transition of phospholipids but also the temperature of the phospholipid phase transition from the tilted gel phase (L ) bÕ to the ripple gel phase (P ). bÕ The results were compared with those obtained with EPR study. EPR study was carried out in the temperature range from 284 to 310 K i.e. below and above the phase transition temperature TC of DMPC. On the basis of EPR spectra of spin marker 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO) incorporated into the liposome, the values of parameters f were determined. Hence TEMPO can be used to observe the change in partition between aqueous and fluid lipid regions. The change in the relative values of f determined for DMPC as a function of temperature shows that this phospholipid undergoes a transition from a Ôgel phaseÕ to a lamellar smectic liquid crystalline phase in the presence of excess water. The EPR study of TEMPO allowed us to determine the transition temperature TC. The results were compared with those obtained with DSC method.
Danuta Pentak, W. W. Sulkowski, Anna Sulkowska, Journal of Thermal Analysis and Calorimetry, Vol. 93 (2008) 2, 471Ð477
B2532 - Thermal and FTIR investigation of freeze-dried protein-excipient mixtures
The effect of excipients on the secondary structure of lyophilized proteins was studied through second-derivative Fourier transform infrared (FTIR) spectroscopic analysis. The glass transition temperature (Tg), denaturation temperature (Td) and moisture content were determined by differential scanning calorimetry (DSC) and thermogravimetry (TG). Tg, Td and the preservation of protein secondary structure were found to be dependent upon the type and amount of the excipient included in the formulation. Meanwhile, the lyophilized proteins easily adsorbed amounts of moisture during storage to reduce their Tgs and stability.
J. Lu, X.-J. Wang, Y.-X. Liu, C.-B. Ching, Journal of Thermal Analysis and Calorimetry, Vol. 89 (2007) 3, 913Ð919
B2531 - A convenient tool for studying the stability of proteins and nucleic acids. Differential scanning calorimetry
The aim of this work is to discuss the thermodynamic properties, obtained by differential scanning calorimetry (DSC), of the thermal transition of proteins and nucleic acids and to analyze these data using statistical thermodynamic relations. The denaturation of the ordered, specific structures of biological macromolecules is a cooperative process and in many cases the macromolecules undergo a two-state transition. Differential scanning calorimetry, giving direct thermodynamic information, has proved to be very useful in clarifying the energetics of macromolecule transitions and in characterizing their thermal stability. Here, various examples are discussed: i) the equilibrium thermal denaturation of ribonuclease A, a model for the use of DSC by following the temperature-unfolding of the proteins, a monomolecular transition; ii) the equilibrium thermal dissociation of a DNA double helix in two strands, an example of how DSC is used to follow a bimolecular process; iii) an example of the use of DSC for studying the melting of unimolecular and tetramolecular DNA quadruple-helices.
Concetta Giancola, Journal of Thermal Analysis and Calorimetry, Vol. 91 (2008) 1, 79Ð85
B2530 - Fractions of thermodynamic functions for native lysozyme adsorption onto moderately hydrophobic surface
Calorimetric measurement of adsorption enthalpies of native lysozyme(Lyz) on a moderately hydrophobic surface at 25¡C, pH 7.0 and various salt concentrations was performed. Based on the thermodynamics of stoichiometric displacement theory (SDT), we calculated the fractions of thermodynamic functions involving four subprocesses during a displacement adsorption process fromthe directly determined enthalpies in combination with adsorption isotherm measurements. The thermodynamic fractions reveal the relative degree of the four subprocesses for contributions to enthalpy, entropy and free energy. The results show that native Lyz adsorption on a moderately hydrophobic surface is an entropy driven process contributed mainly by conformational loss of adsorbed Lyz
X. P. Geng, M. R. Zheng, B. H. Wang, Z. M. Lei, X. D. Geng, Journal of Thermal Analysis and Calorimetry, Vol. 93 (2008) 2, 503Ð508
B2529 - Thermodynamic analysis of denaturated lysozyme folded on moderately hydrophobic surface at 298 K
Both calorimetric determination of displacement adsorption enthalpies DH and measurement of adsorbed amounts of lysozyme (Lyz) denatured by 1.8 mol LÐ1 guanidine hydrochloride (GuHCl) on a moderately hydrophobic packings at 298 K, pH 7.0 and various salt concentrations were carried out. Based on the thermodynamics of stoichiometric displacement theory (SDT) the fractions of thermodynamic functions, which related to four subprocesses of denatured protein refolding on the surface, were calculated and thermodynamic analysis that which one of the subprocesses plays major role for contribution to the thermodynamic fractions was made in detail. The moderately hydrophobic surface can provide denatured Lyz energy and make it gain more conformation with surface coverage or salt concentration increment. The displacement adsorptions of denatured Lyz onto PEG-600 surface are exothermic, more structure-ordered and enthalpy driven processes.
X. P. Geng, H. Gao, B. H. Wang, A. L. Liu, X. Y. Feng, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 2, 345Ð352
B2528 - Thermal stability of DNA in DNAÐinduced DOTAP liposome aggregates
The influence on the melting of calf thymus DNA induced by cationic liposomes, commonly used in gene therapy, was studied by means of ultraviolet spectrophotometry and differential scanning calorimetry. Both the two methods reveal that DNA in DNA-induced liposome complexes undergoes a denaturation process at a much higher temperature than free DNA does. The extent of protection strongly depends on the charge ratio R(+/Ð) of liposomeÐDNA complexes. In the case of dioleoyl trimethyl ammonium propane (DOTAP) liposomes, the maximum of the stabilization occurs at R(+/Ð)=0.7, where the DNA is still native up to temperatures higher than 100¡C. This protection against denaturation up to higher temperatures might be of importance for bio-technological applications, such as biomolecular separation, antigene sequencing and for drug design purpose.
S. Zuzzi, G. Onor, C. Cametti, Journal of Thermal Analysis and Calorimetry, Vol. 93 (2008) 2, 527Ð533
B2527 - Domains in bovine seminal ribonuclease
Bovine seminal ribonuclease is the only pancreatic-type ribonuclease to possess a dimeric structure: the two identical subunits are covalently linked by two disulfide bridges. Actually, the protein exists in two different dimeric structures owing to the possibility of swapping the N-terminal -helical segments: the swapped MxM dimer, and the non-swapped M=M dimer. The thermal denaturation of the two separated forms is investigated by differential scanning calorimetry. The process is reversible and can be represented by two sequential two-state transitions, indicating the presence of two domains in BS-RNase, regardless of the swapping phenomenon. Inspection of the structural models leads to the tentative identification of an external domain and a core domain, the latter more stable
Francesca Catanzano, G. Graziano, Journal of Thermal Analysis and Calorimetry, Vol. 91 (2008) 1, 61Ð66
B2526 - The effect of trimethylamine N-oxide on RNase A stability . A DSC study
The thermal stability of bovine pancreatic ribonuclease (RNase A) has been investigated in the presence of trimethylamine N-oxide (TMAO), a naturally occurring osmolyte, by means of differential scanning calorimetry (DSC) and circular dichroism (CD) measurements at neutral and acid pH conditions. It is well known that compatible osmolytes such as TMAO are effective in stabilizing protein structure and counteracting the denaturing the effect of urea and guanidinium hydrochloride (GuHCl). Calorimetric results show that TMAO stabilizes RNase A at pH 7.0 and does not stabilize the protein at pH 4.0. RNase A thermal denaturation in the presence of TMAO is a reversible two-state N D process. We also show that TMAO counteracts the urea and GuHCl denaturing effect at neutral pH, whereas the counteracting ability is lost at acid pH.
Fabrizia Foglia, Paola Carullo, Pompea Del Vecchio, Journal of Thermal Analysis and Calorimetry, Vol. 91 (2008) 1, 67Ð72
B2525 - Comparative study of DSC pattern, colour and texture of shrimps during heating
Shrimp continues to be the most important commodity traded in value terms, accounting for 16.5% of the total value of internationally traded fishery products in 2004. Despite this importance of shrimp, literature is almost lacking on reports dealing with changes in functional properties and quality caused by heating shrimps while influence of freezing has been investigated more in depth. Therefore, objective of the study was cooking shrimp to different core temperatures in the range 30Ð80¡C and monitoring changes in quality by measuring colour and texture attributes. DSC curves taken on differently heated shrimp differed markedly. With increasing temperature the enthalpy of denaturation decreased significantly.
R. Schubring, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 3, 749Ð757
B2524 - DSC examination of the degenerated human palmar aponeurosis in Dupuytren disease
The Dupuytren contracture Ð degenerative shortening of the palmar aponeurosis Ð is a common disease of the hand in Europe. The aetiology of the degenerative changes in the collagen structures is still not clear. To describe the clinical manifestation of the disease we use an international classification according to Iselin. Our hypothesis was that in Dupuytren disease there is a clear pathological abnormality in the tissue elements building up the palmar aponeurosis, which is responsible for the disease, and could be monitored besides the classical histological methods by differential scanning calorimetry. The thermal denaturation of different parts of human samples was monitored by a SETARAM Micro DSC-II calorimeter. All the experiments were performed between 0 and 100¡C. The heating rate was 0.3 K minÐ1. DSC scans clearly demonstrated significant differences between the different types and conditions of samples (control: Tm=63¡C and ?Hcal=4.1 J gÐ1, stage I.: Tm= 63¡C and ?Hcal=5.1 J gÐ1, stage II.: Tm=64¡C and ?Hcal=5.2 J gÐ1, stage III.: Tm=60¡C and ?Hcal=5.2 J gÐ1, stage IV.: Tm=60.2¡C and ?Hcal=5.3 J gÐ1). The heat capacity change between native and denatured states of aponeurosis samples increased with the degree of structural alterations indicating significant water loosing. These observations could be explained with the structural alterations caused by the biochemical processes. With our investigations we could demonstrate that DSC is a useful and well applicable method for the investigation of collagen tissue of the human aponeurosis. Our results may be of clinical relevance in the future i.e. in the choice of the optimal time of surgical therapy of different clinical level Dupuytren contractures.
N. Wiegand, L. Vmhidy, B. Patczai, E. Dmse, P. Than, L. Kereskai, D. Lrinczy, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 3, 797Ð800
B2523 - DSC examination of the esophagus after implantation of special stents designed for the management of acute esophagus variceal bleeding. Experimental study
Massive bleeding from esophagus varices presents a life threatening complication of portal hypertension. No effective method of treatment is available until now, that would guarantee high grade of patient wellness during the conditioning and investigation phase until the definitive treatment could be introduced. The aim of this study was to evaluate the tissue response to esophagus stents Ð designed for manage acute variceal bleeding Ð in animal experiment. Self-expandable nitinol stents were introduced into the esophagus of six porcines. Another twelve porcines were undergone the same procedure, using the new biodegradable stents made of PDO (polydioxanon). Histological investigations of the stented esophagus segments were observed after 2 and 4 weeks at the first 12 animals. To monitor the time of stent degradation, histology were performed 7 and 12 weeks after the implantation in the biodegradable group (3Ð3 animals). Differential scanning calorimetric examination was performed in all esophagus samples. Focal erosion of the esophagus segments was more explicit in the nitinol group at the histology. On the 7th week all of the biodegradable stent were in the stomach and on the 12th week these were completely solved. DSC examination showed significant alterations in the structure of the esophagus in both stented group compared to the healthy control. This experiment showed that the new self-expandable stents are safety and suitable procedure without deterioration of the esophageal wall. According to our DSC results the thermal denaturation of intact esophagus, its mucosa and muscle fragments revealed significant differences compared to healthy sample in favour the new biodegradable stent. Safety and efficiency in the experimental model had encouraged us to apply this method successfully patients with bleeding esophagus varices. The long term goal is to show that stent placement could be an effective way of decreasing or stabilising the acute bleeding from ruptured esophagus varices in cirrhotic patients.
L. Benk, J. Danis, R. Hubmann, G. Kasza, va Gmri, Erzsbet Rth, D. Lrinczy
B2522 - DSC examination of intestinal tissue following warm ishemia and reperfusion injury
The fact that small bowel is extremely sensitive to ischemia/reperfusion (I/R) injury had encouraged us to compare the conventional histology and differential scanning calorimetry (DSC) methods in intestinal structural changes following experimental warm I/R models. Our histological findings showed that longer warm I/R period caused more severe damage in structure of mucosa and crypts, but there were no changes in the muscular layer. According to our DSC data (transition temperature, calorimetric enthalpy) suggest that the thermal destruction of mucosa, muscular layer and total intestinal wall following I/R injury revealed significant differences compared to normal bowel structure.
Klra Nedvig, Andrea Ferencz, Erzsbet Rth, D. Lrinczy, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 3, 775Ð779
B2521 - Human uterus in pregnancy, as it can be monitored by DSC examination. A preliminary study
The myometrium is the main component in enlargement of uterus and plays essential role in labour contraction. Its physiologic and elastic state has a decisive role in the labour process. We have made the first attempt to find correlation between the thermal parameters of uterus and progress of gravidity. Significant differences were observed between cyclic, non-pregnant and postmenopausal state (0.69 and 0.98 J gÐ1 calorimetric enthalpy as well as 60.6 and 63.1¡C for Tm), as well as among the different gestational stages and complications. In case of twin pregnancy and dystocia we have found extremities: 0.37 and 1.34 J gÐ1 calorimetric enthalpies, with 62 and 61.6¡C melting temperatures. DSC method seems to be promising tool to follow and understand different molecular changes in the myometrium during pregnancy and its complication of human labour.
F. Wilhelm, K. A. Kovcs, Zs. Vrtes, D. Lrinczy, Journal of Thermal Analysis and Calorimetry, Vol. 89 (2007) 3, 863Ð865
B2520 - DSC investigation of early pregnant uterus of the rat
The aim of the present work was the characterization of nonpregnant and early pregnant myometrium (days 3Ð6) of the rat by means of differential scanning calorimetry (DSC). The spontaneous motor activity as well as the KCl-evoked contractions of isolated uterine rings was additionally recorded. A relatively close correlation was found between calorimetric enthalpy (DH) and the contractility of the uterus samples. Our results indicate that DSC is a useful tool for the investigation of the functions of developing myometrium and it can be considered as supplementing the traditional structural and functional methods.
G. Cs'k, I. Zupk--, G. Regdon Jr., G. Falkay, D. Lrinczy, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 3, 695Ð698
B2519 - DSC analysis of human fat tissue in steroid induced osteonecrosis. A preliminary study
Osteonecrosis (ON) of the femoral frequently occurs after steroid medication. One of the final pathways leading to steroid induced ON is thought to be pathologic fat metabolism. The pathobiological mechanism underlying the induction of fat metabolism outslides by steroids leading to ON has not been fully elucidated. The purpose of this study was to examine the intraoperative obtained gluteal fat tissue from ON patients with histology, gas chromatography (GC) and differential scanning calorimetry (DSC) and to compare them with otherwise healthy patientÕs samples. The histological sections showed no significant differences compared with the control group. GC revealed that fraction of saturated fatty acids decreased in ON samples from mean values of controls of 24% to 21, the polyunsaturated fraction from 20 to 14%. The monounsaturated acids showed an increase from mean rate of 52% of the controls to 65% of steroid treated samples. DSC curves correlate with chromatographic analysis of the tissue fatty acids (Steroid treated, heating between 0Ð100¡C: Tm=5.7¡C, ?H= Ð15.8J/gÐ1; heating between Ð20Ð100¡C: Tm= Ð9.96 and 5.85¡C, ?H=Ð59.17 and Ð16.2 J gÐ1. Non-necrotic, heating between 0Ð100¡C: two separable transition with Tm=5.7 and 9.9¡C, total ?H= Ð20.8 J gÐ1; heating between Ð20Ð100¡C: Tm= Ð10.9 and 4.95¡C, total ?H= Ð75.8 J gÐ1.). Our preliminary findings are rather tendentious. Further investigations are needed with higher sample rate and under other anamnestic circumstances too.
G. Bognr, Cs. Pintr, B. Horvth, T. Sydo, E. Ligeti, J. Pulai, D. Lrinczy, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 3, 769Ð774
B2518 - Differential scanning calorimetric examination of the ruptured Achilles tendon in human
The Achilles tendon rupture is a common injury of the foot in middle age and physically active population in Europe. The aetiology of the degenerative changes in the collagen structures of the tendon which could be disposed for the rupture is still not clear. Our hypothesis was that before the injury there is a clear pathological abnormality in the tissue elements building up the Achilles tendon, which is responsible for the disease, and could be monitored besides the classical histological methods by differential scanning calorimetry. The thermal denaturation of human samples was monitored by a SETARAM Micro DSC-II calorimeter. All the experiments were performed between 0 and 100 ?C. The heating rate was 0.3 K/min. DSC scans clearly demonstrated significant differences between the control and ruptured samples (control:Tm = 59.7 ?C, T1/2 = 1.4 ?C and ?Hcal = 8.54 J/g; ruptured: Tm = 62.75 ?C, T1/2 = 2.6 ?C and ?Hcal = 1.54 J/g). These observations could be explained with the structural alterations caused by the biochemical and structural processes. With our investigations we could demonstrate that DSC is a useful and well applicable method for the investigation of collagen tissue of the human Achilles tendon. We can prove with this method, that the earlier series of microtraumas which result a scar formation in the tendon tissue increases the thermal stability of collagen in ruptured tendon.
N. Wiegand, L. Vmhidy, L. Kereskai, D. Lrinczy, Thermochimica Acta 498 (2010) 7Ð10
B2517 - Application of isotherm calorimetry in the development of foods containing probiotic live flora and enriched with bioavailable Ca2+
The development of functional foods of probiotic effect based on the slime-producing strains isolated in the 1980s, and that of enriched with Ca on the utilization of the high Ca-containing whey of the quarg production in the Carpathian basin using fermentation. The probiotic properties of the slime-producing microbe strains isolated have been proved by in vitro and in vivo examinations. We have used an isotherm DSC method to identify the probiotic microbes. The percentile ratio of probiotic and other microbes was determined in the product by this technique. By utilization of quarg whey a special additive food for Ca-enrichment has been developed which is suitable to complete or enrich different foods (dairy, meat and bakery products). The products developed are: probiotic kefir (Synbiofir), probiotic sour cream, probiotic butter cream, poultry meat products completed with Ca, bakery products completed with Ca.
B. Schffer, Beta Keller, D. Lrinczy, Journal of Thermal Analysis and Calorimetry, Vol. 95 (2009) 3, 703Ð708
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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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