Calorimeter characterization

The relationships shown in Section 3.1.3 are also pertinent to large-scale reactors. By using different solvents and volumes of solvent, pilot and production reactor heat transfer characteristics can be determined from a series of experiments. A primary limitation, compared to reaction calorimeter characterization, is that a calibration probe is rarely available. Thus, heat-up and cool-down studies, performed... 

Let us normalize in the dimension of temperature the isoperibol n-n calorimeter characterized by a system of two concentric domains shown in Fig. 4.5 [21, 45]. 

Thermal Analysis - Differential Scanning Calorimetry (DSC) and thermal gravimetric analysis (TGA) were used to characterize the thermal properties of the polymers synthesized. DSC analysis was performed on a Perkin-Elmer Differential Scanning Calorimeter, Model 2C with a thermal analysis data station. Thermal gravimetric analysis (TGA) was carried out on a DuPont thermal gravimeter, Model 951. From the DSC and TGA plots of poly (N-pheny 1-3,4-dimethylene-... 

In the various sections of this article, it has been attempted to show that heat-flow calorimetry does not present some of the theoretical or practical limitations which restrain the use of other calorimetric techniques in adsorption or heterogeneous catalysis studies. Provided that some relatively simple calibration tests and preliminary experiments, which have been described, are carefully made, the heat evolved during fast or slow adsorptions or surface interactions may be measured with precision in heat-flow calorimeters which are, moreover, particularly suitable for investigating surface phenomena on solids with a poor heat conductivity, as most industrial catalysts indeed are. The excellent stability of the zero reading, the high sensitivity level, and the remarkable fidelity which characterize many heat-flow microcalorimeters, and especially the Calvet microcalorimeters, permit, in most cases, the correct determination of the Q-0 curve—the energy spectrum of the adsorbent surface with respect to... 

The main parameter which characterizes a calorimeter is the resolution, whereas in astronomical bolometers the qualifying parameter is the NEP (noise equivalent power, see later). Also the size is very different bolometers are usually very smaller. Their more sophisticated technology allows the realization of large arrays of detectors. In operation, bolometers usually handle a chopped signal (tens of Hertz) of much smaller energy than calorimeters. 

Data may be simple physical properties or sophisticated calorimeter data to characterize two phase flow (including gassy systems and/or high viscosity laminar flow systems). 

Several commercial calorimeters are available to characterize runaway reactions. These include the accelerating rate calorimeter (ARC), the reactive system screening tool (RSST), the automatic pressure-tracking adiabatic calorimeter (APTAC), and the vent sizing package (VSP). Each calorimeter has a different sample size, container design, data acquisition hardware, and data sensitivity. 

The RSST (reactive system screening tool) is a laboratory device used to characterize the reactive nature of liquid materials. It is essentially an adiabatic calorimeter, with the test sample heated at a constant temperature rate until an exothermic reaction is encountered. 

Scottish chemist, physicist, and physician. Professor of chemistry at Glasgow. He clearly characterized carbon dioxide ( fixed air ) as the gas which makes caustic alkalies mild, and distinguished between magnesia and lime. He discovered the latent heats of fusion and vaporization, measured the specific heats of many substances, and invented an ice calorimeter. 

This concept of TMRad was initially developed by Semenov [7] and was reintroduced by Townsend and Tou [8] as they developed the accelerating rate calorimeter (see Section 4.3.1.3). It is used to characterize decomposition reactions, as described in Chapters 3 and 11. 

Adiabatic conditions may be achieved either by a thermal insulation or by an active compensation of heat losses. Examples are the Dewar calorimeter, achieving a thermal insulation [2-4] or the Accelerating Rate Calorimeter (ARC) [5] or the Phitec [6], using a compensation heater avoiding the heat flow from the sample to the surroundings. These calorimeters are especially useful for the characterization of runaway reactions. 

For cases where the secondary reaction plays a role (class 5), or if the gas release rate must be checked (classes 2 or 4), the heat release rate can be calculated from the thermal stability tests (DSC or Calvet calorimeter). Secondary reactions are often characterized using the concept of Time to Maximum Rate under adiabatic conditions (TMRad). A long time to maximum rate means that the time available to take risk-reducing measures is sufficient. However, a short time means that the... 

There is evidence to show that the particle size of the filler also plays a significant role in flammability resistance. For example, below a certain particle size (about 1-2 pm), in many tests, including oxygen index, aluminum hydroxide shows enhanced fire-retarding performance,34 which may be associated with the rate of filler decomposition and/or with the formation of a more stable ash. However, it has been found that the particle size effect is absent, or less evident, in the cone calorimeter test.35 Similarly, particle size reduction has been shown to enhance fire retardancy in magnesium hydroxide-filled PP in this case, samples were characterized by the UL94 test.36 This raises the question as to whether further reductions in particle size to the nanoscale will lead to an additional increase in flammability performance, and perhaps enable filler overall levels to be significantly reduced. This aspect is considered in a later section. 

Of the several approaches that have been used to calculate fuel generation rates from solid materials in CFD-based fire growth calculations, the simplest are empirical models. Instead of attempting to model the physical processes that lead to gaseous fuel production inside decomposing solids, empirical data that can be measured (transient heat release or mass loss rate) or inferred (heat of gasification) from common bench-scale fire tests such as the Cone Calorimeter are used to characterize fuel generation processes. 

A round robin was organized wherein several teams modeled the fire spread before they were provided with the experimental results (a priori simulations) [101]. Participants were given basic information regarding the layout of the apartment and the types of combustibles present, but they were not provided with small-scale test data (i.e., Cone Calorimeter, thermogravimetric analysis, etc.) to characterize any of the combustibles present in the apartment. Most teams used FDS4, and two teams used CFAST. 

The oxide characterization steps are carried out with laboratory equipment that has been adapted as necessary to facilitate handling in-cell with the manipulators. The items include a 210-yin-opening stainless steel screen assembly, a 300-g-capacity triple-beam balance, a 10-mL glass graduated cylinder and assorted weigh pans, spatulas, and oxide containers. A remotely operated calorimeter is used to assay the 244Cm content. 

Electrochemical calorimetry — is the application of calorimetry to thermally characterize electrochemical systems. It includes several methods to investigate, for instances, thermal effects in batteries and to determine the -> molar electrochemical Peltier heat. Instrumentation for electrochemical calorimetric studies includes a calorimeter to establish the relationship between the amount of heat released or absorbed with other electrochemical variables, while an electrochemical reaction is taking place. Electrochemical calorimeters are usually tailor-made for a specific electrochemical system and must be well suited for a wide range of operation temperatures and the evaluation of the heat generation rate of the process. Electrochemical calorimeter components include a power supply, a device to control charge and discharge processes, ammeter and voltmeter to measure the current and voltage, as well as a computerized data acquisition system [i]. In situ calorimetry also has been developed for voltammetry of immobilized particles [ii,iii]. 

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