Page 101 - Gas Adsorption Equilibria
P. 101

2. Volumetry / Manometry                                         87












          Analysis of numerical data shows that measurements of pressures (p, p*), i. e.
          values of         are  the  most crucial for accurate measurements of

          followed of course by temperature  measurements     and those  for basic
          data of the  equipment            and  of the  sorbing material    To
          achieve useful results, i. e.               limiting values of variances
          should     hold     as     follows     [2.7]:




          2.4      Example

             In Figure  2.2  equilibrium  adsorption  data for  carbon  dioxide  on
          zeolite Na 13X (Linde, UOP) are presented for temperatures 298 K and  303
          K.  The mol numbers of the Gibbs  surface  excess amounts per unit mass of
          sorbent are depicted as function of the sorptive gas pressure and temperature.
          Relative     uncertainties    of      measurements      are     about
                            The  subcritical isotherms are  in the  range  of pressure
          measured of Type I – IUPAC classification [2.20].

             However, the adsorption  isotherms  exhibit Type II  structure if  the
          saturation pressure      is approached, cp. Chapter 3. Prior to adsorption,
          the zeolite has been “activated” at 623 K for 3 hours under vacuum conditions
          (p <  15 Pa). Some characteristic data of the zeolite also have been measured
          in our laboratory  [2.19], namely the BET surface at 77 K being
          (UOP-date:              the total pore volume being            the He-
          expansion density being

             Equilibration times varied from 15 minutes at low pressures up to (nearly)
          1 hour  at  the  higher  pressures considered,  i. e.            This
          information was gained from time dependent temperature signals produced by
          the sorbent  sample  and gained simultaneously  with adsorption equilibria
          measurements [2.23], cp. Sect. 5.
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