Isothermal typical experiment

Adsorption is often studied using powders or porous materials because the total surface area is large even for small amounts of adsorbent. In a typical experiment the volume (V) or the mass (to = V/p) adsorbed per gram of adsorbent, is measured. Theoretical models always describe an adsorption per surface area. In order to compare theoretical isotherms to experimentally determined adsorption results, the specific surface area needs to be known. The specific surface area (in m2/kg) is the surface area per kg of adsorbent. Once the specific surface area is known, the area can be calculated by A = madT, where mad is the mass of the adsorbent. 

The results of typical experiments are shown in Figure 6. The isotherms of methanol also obey the Brunauer, Emmett, and Teller equation, as may be judged from the linear plots in the inset of Figure 6. 

A typical quasi isothermal crystallization experiment is shown in Figure 1.23. In a first step, the previous crys-... 

Nitrogen adsorption experiments showed a typical t)q5e I isotherm for activated carbon catalysts. For iron impregnated catalysts the specific surface area decreased fix>m 1088 m /g (0.5 wt% Fe ) to 1020 m /g (5.0 wt% Fe). No agglomerization of metal tin or tin oxide was observed from the SEM image of 5Fe-0.5Sn/AC catalyst (Fig. 1). In Fig. 2 iron oxides on the catalyst surface can be seen from the X-Ray diffractions. The peaks of tin or tin oxide cannot be investigated because the quantity of loaded tin is very small and the dispersion of tin particle is high on the support surface. 

Adiabatic calorimetry. Dewar tests are carried out at atmospheric and elevated pressure. Sealed ampoules, Dewars with mixing, isothermal calorimeters, etc. can be used. Temperature and pressure are measured as a function of time. From these data rates of temperature and pressure rises as well as the adiabatic temperature ri.se may be determined. If the log p versus UT graph is a straight line, this is likely to be the vapour pressure. If the graph is curved, decomposition reactions should be considered. Typical temperature-time curves obtained from Dewar flask experiments are shown in Fig. 5.4-60. The adiabatic induction time can be evaluated as a function of the initial temperature and as a function of the temperature at which the induction time, tmi, exceeds a specified value. 

A survey of the literature shows that although very different calorimeters or microcalorimeters have been used for measuring heats of adsorption, most of them were of the adiabatic type, only a few were isothermal, and until recently (14, 15), none were typical heat-flow calorimeters. This results probably from the fact that heat-flow calorimetry was developed more recently than isothermal or adiabatic calorimetry (16, 17). We believe, however, from our experience, that heat-flow calorimeters present, for the measurement of heats of adsorption, qualities and advantages which are not met by other calorimeters. Without entering, at this point, upon a discussion of the respective merits of different adsorption calorimeters, let us indicate briefly that heat-flow calorimeters are particularly adapted to the investigation (1) of slow adsorption or reaction processes, (2) at moderate or high temperatures, and (3) on solids which present a poor thermal diffusivity. Heat-flow calorimetry appears thus to allow the study of adsorption or reaction processes which cannot be studied conveniently with the usual adiabatic or pseudoadiabatic, adsorption calorimeters. In this respect, heat-flow calorimetry should be considered, actually, as a new tool in adsorption and heterogeneous catalysis research. 

Figure 1 has shown that the maximum chemisorption of oxygen on chars from untreated wood occurs at HTT 450°-500°C. However, in order to understand better the effect of metal ions on the total process consisting of pyrolysis and subsequent chemisorption and oxidation of wood char, it was necessary to carry out pyrolysis, isothermal chemisorption and oxidation reactions in a single experiment. A typical overall pyrolysis, isothermal chemisorption (140°C) and oxidation curve is shown in Figure 2. The temperature program is (1) heat from 25° to 500°C at 5°C/min, (2) cool at...

Typically, adsorption isotherms are generated using a batch experiment at a fixed temperature and a fixed feed composition. These experiments include exposing a known amount of adsorbent to a known concentration of adsorbate at a constant temperature. Once equilibrium is established, the net adsorbate concentration in the liquid is measured. This process is repeated at multiple adsorbate concentrations and temperatures. A plot of adsorbate loading (g adsorbate/g adsorbent) versus adsorbate concentration reveals the adsorption isotherm with the shape of the isotherm determining the suitability of a particular adsorbent for a particular system [20]. 

This experiment is typical of many that are conducted using classical adsorption techniques, such as the measurement of isotherms and control of evacuation temperature and pressure. There is a high probability that such a treatment will increase the number of OH groups on the surface, but there is no direct evidence of this. An improvement could be made if the sample were continuously weighed during the cycle in a vacuum microbalance (160), but even this would not be entirely free from ambiguity. 

Step Transient Experiments at 800 Torr. Activation of pretreated silver was performed under isothermal conditions at 493, 523, and 543 K and 800 torr using a step transient format. A typical spectrum collected at 493 K, obtained by simultaneously pulsing ethylene-d4 and oxygen-18 from separate pulse valves into a continuous helium flow, is plotted in Figure 4. In this example, the oxygen to ethylene ratio was 2 1. As observed in the steady-flow TPSR experiments, the pretreated sample is readily activated, while the preoxidi samples remain inactive. 

Kinetic experiments were carried out isothermally in autoclave reactors of sizes 500 ml and 600 ml. The stirring rate was typically 1500 rpm. In most cases, the reactors operated as slurry reactors with small catalyst particles (45-90 micrometer), but comparative experiments were carried out with a static basket using large trilobic catalyst pellets (citral hydrogenation). Samples were withdrawn for analysis (GC for citral hydrogenation and HPLC for lactose hydrogenation). The experimental details as well as qualitative kinetics are reported in previous papers of our group Kuusisto et al. (17), Aumo et al. (5). 

Determination of the reaction rate from calorimetric measurements, using DSC technique, is very useful and was applied with success for many template polymerization systems and for blank polymerizations.Two types of calorimetric measurements were described isothermal and scanning experiments. The heat of polymerization can be measured by DSC method, measuring thermal effect of polymerization and ignoring the heat produced from decomposition of the initiator and heat of termination. In isothermal experiments sample is placed at a chosen temperature and thermogram is recorded versus time. Assuming typical relationship... 

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