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B2596 - Densities, Viscosities, Heat Capacities, and Vapor Liquid Equilibria of Ammonia + Sodium Thiocyanate Solutions at Several Temperatures
Several thermophysical properties were experimentally measured for the ammonia?sodium thiocyanate mixtures at several temperatures: density from (269.4 to 350.9) K, dynamic viscosity from (269.8 to 369.5) K, and isobaric heat capacity from (304.17 to 364.15) K, all them at a constant pressure of 3 MPa, and vapor liquid equilibria from (253.1 to 393.1) K. All properties were measured in a range of composition from 0.35 to 0.90 in ammonia mass fraction. The experimental techniques used were a vibrating-tube densimeter, a piston-style viscometer, a heat flux Calvet-type calorimeter, and a static method, respectively. The measured data were correlated as a function of temperature and composition using empirical equations and were compared with literature values.
Shrirang K. Chaudhari, Daniel Salavera, Alberto Coronas, J. Chem. Eng. Data 2011, 56, 2861Ð2869
B2595 - Molar Heat Capacity of Aqueous Sulfolane, 4-Formylmorpholine, 1-Methyl-2-pyrrolidinone, and Triethylene Glycol Dimethyl Ether Solutions from (303.15 to 353.15) K
The present study has focused on the experimental measurements of the molar heat capacities of four aqueous physical solvents of importance in natural gas sweetening: (1) tetramethylene sulfone (sulfolane), (2) 4-formylmorpholine (NFM), (3) 1-methyl-2-pyrrolidinone (NMP), and (4) triethylene glycol dimethyl ether (TEGDME). The measurements of the molar heat capacities were carried out in the temperature range of (303.15 to 353.15) K and for the entire range of mole fractions. Fractional deviations of the measured molar heat capacities from literature data were less than 1 %, and at worst 2 %. Molar excess heat capacities were calculated from the measurements and correlated as a function of mole fraction and temperature employing the Redlich-Kister equation. The excess partial molar quantities (Ci o - Ci*) were calculated by extrapolating the reduced excess heat capacity (Cp E/x1x2) function at x1 ) 0 and x1 ) 1.
Mayur Mundhwa, Salaheddin Elmahmudi, Yadi Maham, Amr Henni, J. Chem. Eng. Data 2009, 54, 2895-2901
B2594 - Calorimetric studies of thermochemical heat storage materials based on mixtures of MgSO4 and MgCl2
Attapulgite granulate impregnated with mixtures of MgSO4 and MgCl2 hydrates was investigated for suitability as a composite thermal energy storage material. These mixtures were chosen because of the very different deliquescence relative humidities of the salts. The thermochemical heat storage of these materials was characterized by measurements of isothermal heat of sorption and thermogravimetry (TG). The salt mixtures showed a different sorption behavior compared to pure MgSO4. The reduction of the deliquescence relative humidity of the mixture by the partial substitution of MgSO4 by MgCl2 increases the capacity of condensation and therefore the released heat. The energy density of the composite heat storage material containing a salt mixture of 20 wt% MgSO4 and 80 wt% MgCl2 was 1590 kJ/kg measured by calorimetry (at 30 ¡C/85% RH) with a desorption temperature of 130 ¡C.
K. Posern, Ch. Kaps, Thermochimica Acta, 502 (2010) 73Ð76
B2593 - Simultaneous determination of sorption, heat of sorption, diffusion coefficient and glass transition depression in polymerÐCO2 systems
PolymerÐCO2 interactions dictate the evolution of various phenomena such as sorption of CO2, polymer swelling, and polymer plasticization. The knowledge of key quantities and parameters such as the amount of absorbed gas, the heat of sorption, or the diffusion coefficient is of great importance for a rational design of related processes. We have designed and constructed an apparatus based on the combination of Calvet calorimetry and pressure drop method. This combination allows for the determination of the amount of absorbed CO2, the heat of sorption, the diffusion coefficient of CO2 in the polymer and, finally, the concentration of CO2 that causes plasticization of the polymer at a specific temperature (below the atmospheric glass transition temperature). We describe and propose a methodology for the simultaneous measurement of the four, above mentioned, parameters. The glass transition depression is determined by a novel approach which, in addition, allows for information about the kinetics of plasticization to be derived. New results at 54.3 ¡C and at various pressures are presented for the PMMAÐCO2 system, and wherever possible, compared with literature data and modeled with the NRHB (Non Random Hydrogen Bonding) model and the dual sorption model.
Costas Tsioptsias, Costas Panayiotou, Thermochimica Acta, 521 (2011) 98Ð106
B2592 - Thermochemistry and kinetics of silica dissolution in NaOH aqueous solution
Dissolution of increasing amounts of silica (?-cristobalite) in the same volume of a 4% weight of sodium hydroxide solution was followed by microcalorimetry in a closed cell at temperature up to 130 ¡C. The process led to the formation of a dissolved entity whose formula depends on the Na2O/SiO2 ratio. At the beginning dissolution gave [3Na2O, 4SiO2] entity and when increasing dissolved silica amounts, the latter transforms into [Na2O, 2SiO2]. Kinetic study showed that dissolution starts by a very rapid step with about 10% of the whole heat energy released and continued with a very slow process. Kinetic analysis showed that the latter agrees with two successive silica first-order reactions scheme. The resulting activation energy values are of the same magnitude order of that deduced from the isoconversional model.
Meriem Fertani-Gmati, Mohamed Jemal, Thermochimica Acta 513 (2011) 43-48
B2591 - Kinetics and thermodynamics of the attack of a phosphate ore by acid solutions at different temperatures
A calorimetric study of the kinetics and thermodynamics of the attack of a phosphate ore from Gafsa region (Tunisia) by phosphoric acid and by a mixture of phosphoric acid and sulfuric acids is undertaken at different temperatures. Two samples of the same ore having different grain size have been used. At 25 ¡C, the dissolution enthalpy in phosphoric acid solution equals ?233.6 ± 2.2 J/g for both of the samples. Attack by the mixture of acids is strongly dependent on the solid granulometry. Interpretation of the calorimetric results by Avrami model shows the existence of three domains attributed to phosphate ore dissolution/H2PO4? neutralisation, hemihydrate (HH) precipitation and hemihydrate/dihydrate (DH) transformation. The attack by the acid mixture was performed at higher temperatures and showed in addition the transitional formation of the anhydrous sulfate (AH) at T ³ 55 ¡C, which transforms into dihydrate after the HH/DH transformation.
K. Antar, M. Jemal, Thermochimica Acta 474 (2008) 32-35
B2590 - Experimental and predicted excess molar enthalpies of binary mixtures containing 2,2?-oxybis[propane], benzene, butan-1-ol, 2-methylpropan-1-ol, 2-methyl-2-ene-1-propanol at 303.15 K
Excess molar enthalpies HE have been measured for liquid binary mixtures of 2,2?-oxybis[propane] (diisopropylether ÔDIPEÕ), or, benzene + butan-1-ol, +2-methylpropan-1-ol (isobutanol), +2-methyl-2-ene-1-propanol (isobutenol), +n-heptane at 303.15 K and constant pressure using a C80, Setaram calorimeter. A RedlichÐKister type equation was used to correlate experimental results. These experimental results, along with our previous data on HE of DIPE + benzene, +cyclohexane [1] are used for estimating interaction parameters in DISQUAC, an extended quasi-chemical group contribution model [0010] and [0015].
Sada Didaoui, Ahmed Ait-Kaci, Fluid Phase Equilibria, 299 (2010) 60Ð64
B2589 - Excess molar enthalpies of dibromomethane with acetonitrile, furan and acetophenone at 303.15 K
Excess molar enthalpies HE at 303.15 K using a microcalorimeter have been determined for binary liquid mixtures of dibromomethane (DBM) with acetonitrile, furan and acetophenone over the entire composition range. The excess molar enthalpies values are endothermic for DBM + acetonitrile, and +furan but they are exothermic for the system DBM + acetophenone. The observed values are fitted with the RedlichÐKister equation by means of the least squares method. The excess partial molar enthalpies of the components and have also been evaluated with the help of HE values. The results indicate the existence of specific interactions between all these components.
Atri Deo Tripathi, Thermochimica Acta, 500 (2010) 128Ð130
B2588 - Heat capacity of NaNO2
Heat capacity in solid state was for the sodium nitrite (NaNO2) measured by using two types of calorimeters. The measurements were performed in the temperature range 273.15Ð583.15 K. Three phase changes were observed in this temperature range Ð one melting and two transitions between different structural modifications. Concerning the transitions between structural modifications, the first was observed at 437.2 ± 0.1 K and the second was found at 438.7 ± 0.1 K. Temperature of melting was then determined to be 553.2 ± 0.2 K with the corresponding heat of fusion being equal to 13.9 ± 0.1 kJ mol?1.
L. Kourkova, R. Svoboda, G. Sadovska, V. Podzemna, A. Kohutova, Thermochimica Acta, 491 (2009) 80Ð83
B2587 - Flow calorimetric insight to competitive sorption of carbon dioxide and methane on coal
Flow calorimetric technique was used to obtain information on the additional adsorption of carbon dioxide on two samples of Czech bituminous coal with pre-adsorbed methane. It was found that most of the adsorption sites for CO2 remain unoccupied when the coal surface is saturated by pre-adsorbed methane. The calorimetric measurements then confirmed the displacement ability of carbon dioxide to methane molecules pre-adsorbed on the coal.
Boleslav Taraba, Thermochimica Acta, 523 (2011) 250Ð252
B2586 - EnthalpyÐentropy compensation for n-hexane adsorption on HZSM-5 containing transition metal ions
In this work, the values of entropy changes related to n-hexane adsorption onto ion-exchanged ZSM-5 zeolites were calculated from differential heats, obtained from microcalorimetric experiments. The existence of enthalpyÐentropy compensation effect, evidenced by the linearity of ØDH vs. ØDS plots and characteristic for all investigated ZSM-5 zeolites, was found. In the case of ZSM-5 structure, modifying the zeolite structure by ion-exchange gives rise to changes in the heats of adsorption and adsorption entropy in the same manner. The factors that can influence the appearance of entropyÐenthalpy compensation were discussed. It was found that compensation effect is governed by ion-induced dipole interaction between highly polarizing cationic centres in zeolite and nonopolar n-hexane molecules, and hence, depends on the size, charge and electron configuration of the cation. It was found also that the compensation temperature is in correlation with the number of zeolitesÕ strong acid centres. Contrary to the adsorption of n-hexane on ZSM-5 zeolites, compensation effect was not found for the adsorption of the same gas on faujasite-type zeolites.
R. Hercigonja, V. Rac, V. Rakic, A. Auroux, J. Chem. Thermodynamics 48 (2012) 112Ð117
B2585 - Selective oxidation of gas phase ammonia over copper chromites catalysts prepared by the solÐgel process
Selective gas phase oxidation of ammonia at atmospheric pressure was studied over a series of undoped and doped (Mn, Ag) copper chromites prepared by solÐgel process (SG). The catalysts were characterized by elemental analysis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and by adsorption microcalorimetry (AMC). A comparative study was made with a commercial copper chromite catalyst. The surface of the solÐgel undoped catalyst was found to be enriched in high valence chromium species with respect to the commercial one (Cr6+/Cr3+=0.56 versus 0.39 for commercial catalyst). From XPS, the Cu2+/(Cu¡+Cu+) ratio was the same (ca. 5) in both catalysts but the solÐgel sample, contained twicemore surface copper species (8.3 at.%) than the commercial one (17.6 at.%). Ammonia AMC experiments showed both a higher ammonia uptake and a wider strength distribution of adsorption sites on the solÐgel-prepared sample than on the commercial one. Improved catalytic performance in selective oxidation of ammonia at low temperature was obtained by simultaneous addition of silver and manganese to the solÐgel-prepared copper chromite.
A. Kaddouri, N. Dupont, P. Glin, A. Auroux, Catalysis Communications 15 (2011) 32Ð36
B2584 - AcidÐbase properties of niobiumzirconium mixed oxide catalysts for glycerol dehydration by calorimetric and catalytic investigation
The acidÐbase properties of fresh and used niobiumzirconium mixed oxide catalysts, used for the dehydration of glycerol to acrolein, have been characterized by various techniques. These techniques include ammonia thermoprogrammed desorption (TPD), infrared spectroscopy of absorbed pyridine, and adsorption microcalorimetry of ammonia and sulfur dioxide. Relationships between the catalytic properties and the acidÐbase properties of fresh catalysts have been investigated. The most efficient catalysts were shown to be those for which the zirconia support had a better niobium oxide species covering, but no specific relationship could be established between the acidÐbase, and the selectivity to acrolein. Characterization of the used catalysts showed that the acidic properties of the catalysts had changed considerably with the time spent on stream. No further strong acid sites, and only weak or very weak acid sites were detected. A linear relationship between the total quantity of remaining acidic sites and the rate of glycerol conversion was determined, taking into account an intrinsic activity of the stronger sites, which is more than ten times that of the weaker ones. The deactivation of the catalysts as a function of time on stream has been related to the formation of cyclic molecules, produced by the reaction of acrolein with byproducts resulting from the decomposition of hydroxyacetone and also possibly acrolein and glycerol.
P. LauriolGarbey, G. Postole, S. Loridant, A. Auroux, V. Belliere-Baca, P. Rey, J.M.M. Millet, Applied Catalysis B: Environmental 106 (2011) 94Ð 102
B2583 - New methodology for simultaneous volumetric and calorimetric measurements: Direct determination of ?p and Cp for liquids under pressure
A new batch cell has been developed to measure simultaneously both isobaric thermal expansion and isobaric heat capacity from calorimetric measurements. The isobaric thermal expansion is directly proportional to the linear displacement of an inner flexible below and the heat capacity is calculated from the calorimetric signal. The apparatus used was a commercial Setaram C-80 calorimeter and together with this type of vessels can be operated up to 20 MPa and in the temperature range of 303.15Ð523.15 K, In this work, calibration was carried out using 1-hexanol and subsequently both thermophysical properties were determined for 3-pentanol, 3-ethyl-3-pentanol, and 1-octanol at atmospheric pressure, 5 and 10 MPa, and from 303.15 to 423.15 K in temperature. Finally experimental values were compared with the literature in order to validate this new methodology, which allows a very accurate determination of isobaric thermal expansion and isobaric heat capacity.
L. M. Cass, F. Plantier, D. Bessires, Rev. Sci. Instrum. 80, 124902 (2009)
B2582 - Influence of surface acidÐbase properties of zirconia and titania based catalysts on the product selectivity in gas phase dehydration of glycerol
AcidÐbase properties of zirconia and titania basedmaterialswere investigated by adsorption microcalorimetry of NH3 and SO2 probemolecules. Catalytic performance of the catalystswas also tested in the gas phase dehydration of glycerol with the intention of finding correlations between catalytic activity and surface acidÐbase features. Results show that the number of basic sites directly affects the selectivity in gas phase dehydration of glycerol to produce acrolein. Therefore, in order to realize the target reaction it is necessary to control not only the strength and the amount of the desired sites (acidic ones), but also to hinder as much as possible the number/strength/action of the undesired ones (basic ones).
Du?an Sto?i?, Simona Bennici, Jean-Luc Couturier, Jean-Luc Dubois, Aline Auroux, Catalysis Communications 17 (2012) 23Ð28
B2581 - CeO2ÐNb2O5 mixed oxide catalysts: Preparation, characterization and catalytic activity in fructose dehydration reaction
In this work, ceriaÐniobia mixed oxides have been prepared by coprecipitation. The structural, textural, and surface properties of these materials have been fully characterized using appropriate techniques (lowtemperature adsorptionÐdesorption of nitrogen, thermogravimetric analysis, Xray diffraction analysis (XRD), Xray photoelectron spectroscopy (XPS), Raman spectroscopy and temperatureprogrammed reduction/oxidation (TPR/O)). The acidÐbase properties were estimated by the adsorption of appropriate probe molecules Ð NH3 or SO2 were used to estimate the population, strength and strength distribution of acid or basic sites, by means of adsorption microcalorimetry. The nature of acidic sites was determined through the adsorption/desorption of pyridine, studied by infrared spectroscopy. New phases between the oxides were not formed, while there is evidence of interaction between them, as revealed by XRD and Raman spectroscopy. All investigated mixed oxide samples are amphoteric and possess redox centers on their surface. Both redox and acidÐbase properties are dependent on the ratio of ceria to niobia in the samples. Both Lewis and Brnsted acid sites are present on the surface of the mixed oxides. In order to check catalytic abilities of these materials, reaction of fructose dehydration has been performed. All the investigated materials are catalytically active in fructose dehydration; conversion of fructose and selectivity to 5hydroxymethylfurfural (5HMF) improved with increasing content of niobia in the samples.
Dusan Stosic, Simona Bennici, Vesna Rakic, Aline Auroux, Catalysis Today (2011)
B25802 - Excess Molar Enthalpies for the Binary and Ternary Mixtures of Cyclohexane, Tetrahydropyran, and Piperidine at 308.15 K and Atmospheric Pressure: Experimental Measurements and Correlations
Excess molar enthalpies for the binary and ternary mixtures of cyclohexane, tetrahydropyran, and piperidine have been measured using a Calvet microcalorimeter at 308.15 K and atmospheric pressure. All of the binary and ternary systems show endothermic behavior. The experimental binary results are correlated using the Redlich?Kister equation. The excess molar enthalpies for the ternary mixture are correlated using the Cibulka equation. The capability of an artificial neural network algorithm to model these data is finally studied.
Farid B. Belaribi, Ghe?nima Boukais-Belaribi, Amir H. Mohammadi, Dominique Richon, J. Chem. Eng. Data, 2010, 55 (1) 303Ð307
B2579 - Investigation of the WO3/ZrO2 surface acidic properties for the aqueous hydrolysis of cellobiose
A series of WOx/ZrO2 with various tungsten oxide loadings (1Ð20) wt.% was prepared by co-precipitation. The catalysts were characterized by XRD, BET, XPS, Raman spectroscopy, TPR, ammonia adsorption microcalorimetry and pyridine FT-IR spectroscopy. XRD and Raman results showed that the ZrO2 support is predominantly present in the monoclinic phase when the WO3 loading was less than 5 wt.% and predominantly in the tetragonal phase above 10 wt.%. No formation of bulk WO3 was detected for the catalysts calcined at 700 ¡C, which is also the case for the highest loaded samples. TPR results revealed that isolated WO3 species are easier to reduce than amorphous WOx. The ammonia adsorption microcalorimetric study evidenced acid sites with adsorption heats in the range 90bQdiffb130 kJ.mol?1, in amounts which increase with increasing WO3 loading until reaching the monolayer. Concerning the acid site nature, a progressive increase of the amount of Br¿nsted sites with the WO3 loading was observed. The catalytic reaction of cellobiose disaccharide hydrolysis showed a better catalytic performance on the highest WO3 loaded catalysts, associated to the presence of Zr-stabilized WOx clusters and a strong protonic acidity.
R. Kourieh, S. Bennici, M. Marzo, A. Gervasini, A. Auroux, Catalysis Communications 19 (2012) 119Ð126
B2578 - Evaluation of Various Solid Biomass Fuels Using Thermal Analysis and Gas Emission Tests
Various recently proposed biomass fuels are reviewed from the point of view of their safety. Many biomass materials are proposed for use as fuels, such as refuse derived fuel (RDF), wood chips, coal-wood mixtures, etc. However, these fuels have high energy potentials and can cause fires and explosions. We have experienced many such incidents. It is very difficult to extinguish fires in huge piles of biomass fuel or storage facilities. Here current studies on heat generation for these materials and proposed evaluation methods for these new developing materials in Japan are introduced, which are consistent with measurements using highly sensitive calorimeters such as C80, or TAM, and gas emission tests. The highly sensitive calorimeters can detect small heat generation between room temperature and 80 ¡C, due to fermentation or other causes. This heat generation sometimes initiates real fires, and also produces combustible gases which can explode if fuel is stored in silos or indoor storage facilities.
Hiroshi Koseki, Energies 4 (2011) 616-627
B2577 - Study of Enhanced Fine Coal De-sulphurization and De-ashing by Ultrasonic Flotation
The feasibility of using ultrasound to enhance the performance of de-sulphurization and de-ashing during slime flotation was investigated. The Setaram C80 calorimeter, the contact angle gauge DCAT21 and an electrophoresis apparatus were used to study the surface nature of coal, pyrite and refuse before and after ultrasonic conditioning. The yield, ash and sulfur contents of equally sized coal slimes were also measured before and after ultrasonic conditioning. The results show that ultrasonic conditioning can drive the separation of pyrite and refuse from coal. After ultrasonic conditioning the hydrophobicity of coal and hydrophilicity of pyrite and refuse increase. The perfect index of flotation, the perfect index of de-sulphurization and the percentage of de-sulphurization increase by 22.51%, 25.36% and 2.49%, respectively. This study shows that ultrasonic conditioning can enhance the performance of de-sulphurization and de-ashing of coal flotation methods.
Kang Wen-ze, Xun Hai-xin, Chen Jun-tao, J China Univ Mining & Technol 2007, 17(3) 358Ð362
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