Setaram heat flux calorimeter

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). 

Any good-quality heat-flux calorimeter or isothermal titration calorimeter, such as those marketed by TA Instruments (USA) and the associated company Thermometric (Sweden), CSC (USA), Microcal (USA) or Setaram (France). 

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. 

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