Page 153 - Principles of Catalyst Development
P. 153

CATALYST  CHARACTERIZATION                                      141
           confusion in catalysis. Here we adopt the procedures ofthc! ASTM Commit-
           tee.(I93)  There  are  four  major  definitions  of density:  theoretical,  skeletal,
            particle, and packing.


            7.3.1.1.  Theoretical Density
                This is defined as the ratio of the mass of a collection of discrete pieces
           of solid to the sum of the volumes of each piece, if the solid has an ideal
           regular arrangement at the atomic level. Theoretical volumes are determined
            from x-ray diffraction unit cell measurements, so this density is also known
           as the x-ray or unit cell density. Ideal volumes are of little!  use in catalysis,
           and this term  has hardly any applicability.

            7.3.1.2.  Skeletal Density

                In this density, volume is defined as the sum of the volume of the solid
           material  and  any  closed  pores  within. the  solid.  These  pores  cannot  be
            penetrated by any fluid  and become part of the powder volume. A mass of
           catalyst  is  placed  in  a  flask  of known  volume,  and the  amount of helium
            needed to fill  the flask  measured, giving the powder volume by difference.
           Care should be taken to dehydrate all pores thoroughly. Because helium is
           used  as  the  displacing  fluid,  this  density  is  sometimes  called  the  helium
           density.  See Table 7.1  for an example of typical values.

            7.3.1.3.  Particle  Density

                Here the volume  is  the sum  of the solid, closed  pores, and accessible
           pores  within  the  particle.  It is  essentially  the  volume  of the  particle,  but
           should not be found by measuring dimensions. A displacement pychometer
           is  used  but  with  a  fluid  that  does  not  penetrate  the  interior pores  of the
           pellet. One approach is to fill these pores with the fluid prior to displacement,
           for example, with methanol. A more satisfactory method is to use mercury,

                       TABLE 7.1.  Example of Densities 7 wt %  NiOI AI 20 3

                        Density                  Value
                     Theoretical,  d,   3.89 g cm -·3  (crystal)
                     Skeletal, d,      2.39 g em -3  (solid + closed peres)
                     Particle, d"      1.22 g cm- 3  (pellet)
                     Packing, d"       0.732 g cm -3  (bed)
                                       E  =  0.40
                                       ()  =  0.49
   148   149   150   151   152   153   154   155   156   157   158