Calorimeter Setaram

Chemical composition was determined by elemental analysis, by means of a Varian Liberty 200 ICP spectrometer. X-ray powder diffraction (XRD) patterns were collected on a Philips PW 1820 powder diffractometer, using the Ni-filtered C Ka radiation (A, = 1.5406 A). BET surface area and pore size distribution were determined from N2 adsorption isotherms at 77 K (Thermofinnigan Sorptomatic 1990 apparatus, sample out gassing at 573 K for 24 h). Surface acidity was analysed by microcalorimetry at 353 K, using NH3 as probe molecule. Calorimetric runs were performed in a Tian-Calvet heat flow calorimeter (Setaram). Main physico-chemical properties and the total acidity of the catalysts are reported in Table 1. 

The specific heat of InN was measured using InN microcrystals obtained by the microwave nitrogen plasma method [20]. The specific heat was obtained using differential scanning calorimeter Setaram DSC 92 with a precision better than 1% for the entire temperature range the results of these measurements are listed in TABLE 3. 

The enthalpies of fusion of K2TiFe and K3TiFy were determined by AdamkoviCova et al. (1995a,b) using the high-temperature calorimeter Setaram HTC 1800K. The calorimeter was in the DSC mode at scanning rate of 1 K min The sample was sealed in a platinum crucible and placed in the upper alumina cmcible of the calorimetric cell. 

Mixing calorimetry above 1200K. For temperatures above 1200K, different calorimeters should be used because of construction material restrictions. Due to considerable difficulties with the homemade calorimeters, in the majority of cases, commercial equipment is used. One of the most widespread devices working up to 1800 K is the calorimeter Setaram. The whole calorimetric assembly comprise the following parts. 

Figure 4.9. Vertical section of the high-temperature calorimeter Setaram. See text for description.

The heats of complex formation were measured in a Tian-Calvet-Calorimeter (Setaram, Lyon). The electron micrographs were obtained using an electron microscope Hitachi H 500. 

Hahn et al. (1990) measured the excess enthalpy of binary liquid systems with a commercial Picker calorimeter (Setaram, France unfortunately, this is not available anymore) with a precision of about 2%. 

Other instruments include the Calvet microcalorimeters [113], some of which can also run in the scanning mode as a DSC. These are available commercially from SETARAM. The calorimeters exist in several configurations. Each consists of sample and reference vessels placed in an isothermally controlled and insulated block. The side walls are in intimate contact with heat-flow sensors. Typical volumes of sample/reference vessels are 0.1 to 100 cm3, The instruments can be operated from below ambient temperatures up to 300°C (some high temperature instruments can operate up to 1000°C). The sensitivity of these instruments is better than 1 pW, which translates to a detection limit of 1 x 10-3 W/kg with a sample mass of 1 g. 

A heat-flow calorimeter of Tian-Calvet type from Setaram maintained at a desired temperature, from room temperature up to 400°C, was used in connection with a volumetric apparatus equipped with a Me Leod gauge. Sample weights were typically 100 mg and ammonia doses 0.1 cm NTP. 

In the CSM laboratory, Rueff et al. (1988) used a Perkin-Elmer differential scanning calorimeter (DSC-2), with sample containers modified for high pressure, to obtain methane hydrate heat capacity (245-259 K) and heat of dissociation (285 K), which were accurate to within 20%. Rueff (1985) was able to analyze his data to account for the portion of the sample that was ice, in an extension of work done earlier (Rueff and Sloan, 1985) to measure the thermal properties of hydrates in sediments. At Rice University, Lievois (1987) developed a twin-cell heat flux calorimeter and made AH measurements at 278.15 and 283.15 K to within 2.6%. More recently, at CSM a method was developed using the Setaram high pressure (heat-flux) micro-DSC VII (Gupta, 2007) to determine the heat capacity and heats of dissociation of methane hydrate at 277-283 K and at pressures of 5-20 MPa to within 2%. See Section 6.3.2 for gas hydrate heat capacity and heats of dissociation data. Figure 6.6 shows a schematic of the heat flux DSC system. In heat flux DSC, the heat flow necessary to achieve a zero temperature difference between the reference and sample cells is measured through the thermocouples linked to each of the cells. For more details on the principles of calorimetry the reader is referred to Hohne et al. (2003) and Brown (1998). 

The Calvet calorimeters have their roots in the work of Tian [26] and the later modifications by Calvet [7]. Presently this calorimeter type is commercially available from Setaram and the models C80 and BT215 are particularly well adapted for safety studies. It is a differential calorimeter that may be operated isothermally or in the scanning mode as a DSC in the temperature range from room temperature to 300°C for the C80 and -196 to 275°C for the BT215. They show a high... 

CALORIMETRIC MEASOREMEMTS Solution calorimetry was performed at 298.2 0.1 K by using a C-80 differential flux calorimeter manufactured by Setaram. The energy equivalent of the calorimetric signal was determined by electric calibration. The reliability of the equipment was checked by the dissolution of tris-(hydroxymethyl) aminomethane (THAM). Agreement within 0.4% with the published value of +17.75 kJ. mol-1 ( 21) was obtained. 

Immersion calorimetry measurements were carried out with a C80 calorimeter from SETARAM. Before the measurement, the samples were outgassed at 523 K during 4h to a final pressure of lO -lO" Torr. Calorimetric experiments were performed at 297.6 K. 

It should be noted that, in principle, all the flow calorimeters discussed here are capable of operating both in the gas/vapour phase and in the solution phase. However, the calorimeters manufactured by Setaram and Thermometric are generally used for solution-phase studies, whereas the Microscal instruments are designed specifically to facilitate gas/vapour-phase studies. For the purposes of this discussion, gaseous-phase flow calorimetry will centre around a consideration of the Microscal instruments, and solution-phase calorimetry will centre around the Setaram and Thermometric instruments. 

The acid-base properties of the samples were investigated using adsorption of appropriate probe molecules, namely ammonia and sulfur dioxide, monitored by microcalorimetry. The microcalorimetric studies were performed at 353 K for sulfur dioxide adsorption and at 423 K for ammonia adsorption in a heat flow calorimeter of Tian-Calvet type (Setaram C80), linked to a conventional volumetric apparatus. Before each experiment the samples were outgassed overnight at 673 K. 

A Setaram C80 differential microcalorimeter coupled to an evacuable glass gas-handling system was used to monitor ammonia adsorption and associated enthalpies of adsorption. Catalyst samples (ca. 150 mg dry weight) were conditioned in the calorimeter at 100 °C under vacuum for two hours, with an empty reference cell. Successive pulses of ammonia (ca. 0.06 mmol) were introduced to the sample at 100 °C. Enthalpy changes associated with each dose were converted to molar enthalpies of adsorption and are expressed as functions of resin coverage. Further details of the technique have been reported previously. ... 

FIGURE 3.1 Measurement of the cure enthalpy using a DC calorimeter. Isotherms at 180°C the one obtained with the fresh rubber, the other with the already cured rubber (Figure 11, private paper SETARAM from P. Le Parlouer and J. M. Vergnaud). 

A calorimeter C 80 (SETARAM) run in scanning mode with a heating rate of 0.2°C/min. The heat flux is recorded as a function of temperature and time. Samples around 6 g are placed into a cylindrical holder with an internal diameter of 1.7 cm. Two holders are placed into the heating block, one containing the reactive sample, the other alnmina. 

A calorimeter C 80 (SETARAM) is run in scanning mode with a heating rate of 0.2°C/min for measuring the enthalpy of cure. 

A comprehensive experimental research program to investigate the effects of pressure on the products of steam gasification of biomass is currently underway. A stainless steel, tubular microreactor similar to the quartz reactor described earlier has been fabricated for the experimental work. The pyrolysis furnace used with the quartz reactor system has been replaced in the pressurized steam system by a Setaram Differential Scanning Calorimeter (DSC). The DSC provides for quantitative determination of the effects of pressure on pyrolysis kinetics and heats of reaction. 

The SETARAM C 80 calorimeter is particularly well adapted for the investigation of thermal storage reactions. It is a modern type of Calvet microcalorimeters with a large sample volume (Fig. 1) (2). 

Setaram C80 heat flow calorimeter sample mass, polyisocyanate 264 mg, polyol 292 mg crucible, mixing cell with metallic membrane isothermal at 80 °C, sensitivity 1 jiV. Initially, the two reagents are isolated by a membrane and stabilized in the calorimeter at 80 °C. The membrane is cut, and mixing is effected by manual rotation of the stirrer. 

Setaram C80 calorimeter sample mass 3.895 g (use larger amounts of samples to ensure good homogeneity between resin and hardener) standard vessel (a glass tube is introduced into the vessel in order to make the cleaning of the vessel easier) heating rate 0.5 °C min. ... 

Setaram micro DSC-III calorimeter cooling and heating rate 0.5 °C min sample mass ca 900 mg Nj atmosphere. 

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