Adsorption and desorption isotherms by continuous flow

To construct the adsorption isotherm, the adsorption, desorption, and calibration cycle shown in Fig. 15.11 is repeated for each data point required. Errors are not cumulative since each point is independently determined. Relative pressures corresponding to each data point are established by measuring the saturated vapor pressure using any of the preceding methods or by adding 15 torrs to ambient pressure. Thus, if X is the mole fraction of adsorbate in the flow stream, the relative pressure is given by 

The method used to construct the adsorption isotherm cannot be used to build the desorption isotherm. This is true because each data point on the adsorption curve reflects the amount adsorbed by a surface initially free of adsorbate. The desorption isotherm, however, must consist of data 

To scan the hysteresis loop from the adsorption to the desorption isotherm, the sample, immersed in the coolant, is equilibrated with a gas mixture with a relative pressure corresponding to the start of the scan on the adsorption isotherm. The adsorbate concentration is then reduced to a value corresponding to a relative pressure between the adsorption and desorption isotherms. When equilibrium is reached, as indicated by a constant detector signal, the coolant is removed and the resulting desorption signal is calibrated. Repetition of this procedure, each time using a slightly different relative pressure between the adsorption and desorption isotherms, yields a hysteresis scan from the adsorption to the desorption isotherm. 

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