22 Unit Operations of Particulate Solids

with a digital counter. The method will measure the true particle density if
the particles have no closed pores or the apparent particle density if there are
any closed pores, because the volume measured normally excludes any open
pores. If, however, the open pores are filled either by wax impregnation or by
adding water, the method will also measure the envelope volume. By difference
between the two volumes measured the open-pore volume will be
obtained, and can be used as a measure of porosity. Materials that are not
surface-active and incompressible, can be measured using room air and following
the standard procedure that exposes the sample to air pressures from
1 to 2 bar. Compressible materials, however, would need to be tested at lower
pressures (1/2 to 1 bar), while surface-reactive materials may be tested using
helium or another inert gas, because they tend to absorb some or all of the air
constituents. Considering all the aspects involved in the operation of air pycnometers,
densities of most inorganic materials can be reliable determined
using the standard procedure with normal air because their particles are
normally hard and rigid.
The effective particle density is based on the average density within an
aerodynamic envelope around it, including, therefore, any open or closed
pores in the considered volume. One obvious way to measure the volume of
the open pores is using a mercury porosimeter, but this is only suitable for
coarse solids and the necessary equipment is very expensive. Alternative
choices include the bed voidage method, the bed pressure drop method, and
the sand displacement method. The bed voidage method (Abrahamsen and
Geldart, 1980) is based on the observation that the minimum packed voidage
is virtually the same for particles of similar size and particle shape. The procedure
consists on pouring a small amount (0.2–0.25 kg) of a control powder
of known particle effective density into a measuring cylinder and tapping it
to its minimum volume, corresponding to the maximum bulk density. This
procedure is repeated with the unknown powder, or several control powders
in an ideal context. If the porosity after tapping is assumed to be the same for
the control and unknown powders, then their effective densities are in the
same ratio as their bulk densities. The bed pressure method is based on making
measurements of bed pressure drop as a function of gas velocity at two
voidages, when gas is passed through the bed of powder in the laminar flow
regime. The bed is first fluidized to get it well mixed and then gently settled
to its maximum voidage. Pressure drop is measured for at least four velocities;
the bed is then tapped in order to reach as low voidage as possible and
more measurements are made. Calling the set of measurements conditions 1
and 2 respectively, s the gradient of pressure drop, ρb the bulk density, and ρp
the particle density, it can be shown (using the well-known Carman–Kozeny
equation) that a basic relationship can be derived as follows:

The amplitude of the vibration is set so that the powder will fill the cup in
20–30 s. The excess powder is skimmed from the top of the cup using the
sharp edge of a knife or ruler, without disturbing or compacting, the loosely
settled powder.
Poured density is widely used, but the measurement is often performed in
a manner found suitable for the requirements of the individual company or
industry. In some cases the volume occupied by a particular mass of powder
is measured, but the elimination of operation judgment, and thus possible
error, in any measurement is advisable. To achieve this, the use of a standard

discussed in this section, whereas the latter will be included under the general
scope of processing operations, in a subsequent part of this text.
Sone (1972) reported the following compressibility relationship, by tapping,
for food powders:
γn
V Vn
V
abn
bn
=−=+
0
0 1
(1.13)
where γn is the volume reduction fraction, V0 is the initial volume, Vn is the
volume after n taps, and a and b are constants.
The applicability of Equation 1.13 was tested through its fit to the following
linear form:
n
ab
n
na γ = + 1
(1.14)
The constant a in Equations 1.13 and 1.14 represents the asymptotic level of
the volume change or, in other words, the level obtained after a large number
of tappings or a long time in vibration. The constant b is representative of the
rate at which this compaction is achieved, that is, 1/b is the number of vibrations
necessary to reach half of the asymptotic change. In general, this form
of data presentation is very convenient for systems comparisons since it only
involves two constants.
A very common undesirable aspect of compressibility is its negative influence
on flowing capacity. Compression tests have been used widely in pharmaceutics,
ceramics, metallurgy, civil engineering, and in the food powder
field, as a simple and convenient technique to powder compressibility and
flowability.
The pressure–density for powders in a compression test at low-pressure
range can be described by the following equation (Barbosa-Canovas et al.,
1987):
ρσρ
ρσ()0
0
− = + a blog
(1.15)
where ρ(σ) is the bulk density under the applied normal stress σ, ρ0 is the
initial bulk density, and a and b are constants. The constant b represents,
specifically, the compressibility of a given powder. Compression tests are
useful in characterizing the flowability of powders because the interparticle
forces that enable open structures in powder beds succumb under relatively
low pressures. As shown in Equation 1.15, the constant b representing the
change in bulk density by the applied stress is referred to as the powder
compressibility. It has been found that b can be correlated with cohesion of a
variety of powders and therefore could be a simple parameter to indicateflowability changes (Peleg, 1977).
Generally, the higher the compressibility
the poorer the flowability, but if quantitative information about flowability is
required, shear tests are necessary (Schubert, 1987).
One of the standard methods to evaluate the flowability of a particulate
system is to calculate the Hausner ratio after tapping. The Hausner ratio is
defined as the ratio of a powder system’s initial (loose) bulk density to its
tapped bulk density (i.e., the ratio of loose volume to tapped volume). It is
easy to calculate the Hausner ratio and evaluate the flowability when the
loose and tapped volumes of the test material are known. For a Hausner ratio
of 1.0–1.1, the powder is classified as free flowing; 1.1–1.25, medium flowing;
1.25–1.4, difficult flowing; and >1.4, very difficult flowing (Hayes, 1987).
Adding small amounts of fine powders is often used to improve the flow
properties of powdered materials in the chemical, pharmaceutical, and food
industries. In this case, the fine particles coat the coarser particles of the main
constituent and prevent them sticking together. Damp or sticky solids, which
are difficult to handle, may be converted into free-flowing after the added
fine powders absorb small quantities of liquids. Another way to improve
flowability of food powders is by using the agglomeration process, which is
accomplished by wetting the fine particles in an atmosphere of water or suitable
solvent droplets, causing them to collide and stick together, and then
drying the agglomerated material in an air stream. Apart from improving
flowability, agglomerated powders may show better wettability and dispersibility
in liquids, and tend to be dust-free (Hoseney, 1994). Agglomeration
will be discussed further in Chapter 5 of this text.
Reconstitutability is the term used to describe the rate at which dried
materials pick up and absorb water reverting to a condition which resembles
the undried material, when put in contact with an excessive amount of this
liquid (Masters, 1976). In the case of powdered dried biological materials, a
number of properties may influence the overall reconstitution characteristics.
For instance, wettability describes the capacity of the powder particles
to absorb water on their surface, thus initiating reconstitution. Such a property
depends largely on particle size. Small particles, representing a large
surface area-to-mass ratio, may not be wetted individually. In fact, they may
clump together sharing a wetted surface layer. This layer reduces the rate at
which water penetrates into the particle clump. Increasing particle size and/
or agglomerating particles can reduce the incidence of clumping. The nature
of the particle surface can also affect wettability. For example, the presence
of free fat in the surface reduces wettability. The selective use of surface
active agents, such as lecithin, can sometimes improve wettability in dried
powders containing fat. Another important property is the sinkability, which
describes the ability of the powder particles to sink quickly into the water.
This depends mainly on the size and density of the particles. Larger, more
dense particles sink more rapidly than finer, lighter ones. Particles with a
high content of occluded air may be relatively large but exhibit poor sinkability
because of their low density. Finally, dispersibility describes the ease