.

Powder Technology 102 1999 151165

The use of bulk density measurements as flowability indicators
E.C. Abdullah
)
, D. Geldart
Department of Chemical Engineering, Uniersity of Bradford, Bradford, West Yorkshire BD7 1DP, UK
Received 31 March 1998; accepted 28 August 1998
Abstract
Two equipments for measuring the bulk density of powders have been used to assess the flowability of porous and non-porous
powders in which particle size changes as a result of controlling the percentage of fine components in the mixtures. The Hosokawa
Powder Tester, which measures the aerated and tapped bulk densities, gives accurate measurements of bulk density because a fixed
volume of powder is used and the mass of the powder can be measured accurately. On the other hand, the Copley Tap Density
Volumeter, which uses a fixed mass of powder, gives inaccurate measurements due to the difficulty of reading the volume from the
graduated cylinder. Generally, the flowability of powder increases with the increase of particle size, and there appears to be a critical size
range above which flowability does not show any improvement. The packing of particles in two conditions, i.e., aerated and tapped, is
examined and compared with the ideal packing of binary mixtures spherical particles. q1999 Elsevier Science S.A. All rights reserved.
Keywords: Bulk density; Flowability; Critical size range
1. Introduction
The bulk density of a powder is its mass divided by the
volume occupied by the powder. It is also referred to as
the mass of powder that can be packed into a specific
volume. The volume includes the spaces between particles
as well as the envelope volumes of the particles them-
selves. The bulk density of a powder changes tremen-
dously depending on the way particles are packed, like
compaction, consolidation, etc. Therefore there is no unique
value for a given powder.
There are two basic methods of evaluating the bulk
density of a powder that provide a guide to its flow
characteristics.
. .
1 The aerated bulk density random loose packing of
a powder is determined by allowing the dispersed powder
to settle in a container under the influence of gravity. A
powder with a strong structural strength will resist collapse
when dispersed in a container and will have a low bulk
density, while a structurally weak powder will collapse
easily and have a high bulk density. High friction between
the particles results in a low apparent bulk density. With
decreasing friction, the bulk density increases. Svarovsky
)
Corresponding author. Department of Chemical Engineering, Univer-
sity of Malaya, 50603 Kuala Lumpur, Malaysia. Tel.: q60-3-7595206;
Fax: q60-3-7595319
w x
1 defined aerated density as density measured when the
particles are separated from each other by a film of air, and
that, on the whole, they are not in direct contact with each
other. However, most workers interpret it as the bulk
density after the powder has been aerated and allowed to
settle gently, which means the most loosely packed bulk
density.
. .
2 The tapped bulk density random dense packing is
obtained by tapping the container holding the aerated
sample. The structure of a cohesive powder will collapse
significantly on tapping while the weak or free-flowing
powder has little scope for further consolidation. The
powder particles are forced to jump and to lose contact
with each other for a moment while tapping. When there is
reduced friction between the particles, the particles rear-
range and thus tapping results in improved packing condi-
tions.
The ratio of the tapped bulk density to aerated bulk
density is called the Hausner ratio, a term coined by Grey
w x
and Beddow 2 , which is a useful measure of cohesion.
w x
Dutta and Dullea 3 regarded a drop in the Hausner ratio
as a decrease in cohesiveness of the powder.
Generally, there are two types of packing, ordered and
random. Ordered packing is packing where the particles
occupy specific sites with respect to each other such that
long-range order exists as in a crystal structure. On the
other hand, random packing is packing of particles without
0032-5910r99r$ - see front matter q 1999 Elsevier Science S.A. All rights reserved.
. PII: S0032- 5910 98 00208- 3
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 152
order and can be subdivided into two types, based on the
procedure used in assembling the packing, namely, ran-
dom dense packing and random loose packing. Random
dense packing is defined as a random packing where the
particles have been agitated to attain the closest packing
possible without introducing long-range order or deforma-
tion, and is equivalent to the tapped bulk density. Random
loose packing is defined as the packing of particles poured
into a container without agitation or vibration, representing
the lowest stable packing density without introducing
long-range order or deformation, and is equivalent to the
w x
aerated bulk density 4 .
2. Literature survey
The term Hausner ratio was taken from the work of
w x
Hausner 5 , who measured the aerated and tapped density
of three copper powders of similar particle size distribution
but having different shapes, i.e., spherical, irregular and
flake. He found that the further the particle shape deviated
from spherical the higher the ratio of the tapped to the
aerated density for the bulk powder tested. Further tests
with tungsten powders showed that this ratio decreased
with increasing particle size. Friction conditions between
powder particles can be altered by changes with respect to
the particle surfaces, by additions to the powder, such as
lubricants, and by the medium which surrounds the parti-
cles. He also performed tests with two types of electrolytic
.
iron powder, i.e., one with an oxide film as is and the
.
other with clean surfaces as reduced . The results con-
firmed that the powder with an oxide film had a higher
aerated density, which indicates lower friction than is the
case for powder with clean surfaces.
The Hausner ratio is now widely used in industry as a
w x
characterisation property. Harnby et al. 6 mentioned that
the significance of bulk density lies not so much with its
absolute value, but more with the relative changes in bulk
density which occur in response to slight changes in the
characteristics of bulk constituent particles within the pro-
cess. Relative changes in bulk density can be very sensi-
tive indicators of changes in the structural strength of a
loosely compacted powder and hence of its flow character-
istics in many process operations.
w x
Yu and Hall 7 used the funnel method as was also
w x
described in Ref. 1 to measure the aerated density, in
which the powder sample was slowly poured into a stan-
dard funnel with an opening of 5 mm in diameter, through
which the powder flowed and filled a cylindrical container
of height 60 mm and diameter 30 mm. The tapped density
was measured by manual vertical tapping until there was
no change in the height observed. They concluded that the
Hausner ratio is a useful parameter reflecting the particle
particle friction. They have also applied the Heckel equa-
w x w x
tion 8 and Kawakita equation 9 to predict the relation-
ship of packing density and the number of taps. The
Heckel equation and the simplified Kawakita equation are
. .
shown in Eqs. 1 and 2 , respectively.
n
y
.
T
r sr y r yr e 1 . .
n ` ` BA
r
BA
r s 2 .
n
nb r yr .
` BA
1y
1qnb r .
`
w x
Velasco Antequera et al. 10 measured the Hausner
ratio by placing a 100 g sample in a 250 ml graduated
.
cylinder and determined the occupied volume V . After
o
10 and 500 taps, the occupied volumes are determined, V
10
and V , respectively. They calculated the Hausner ratio
500
w x.
and compressibility index introduced by Carr 11 using
the mean value of 10 measurements.
In evaluating the packing characteristics of large non-
cohesive mono-sized and non-spherical particles, Zou and
w x
Yu 12 found that the Hausner ratio decreased with the
increase of sphericity, as given by HRs1.478=10
y0.136C
,
w x
where C is the sphericity of the particle. Geldart et al. 13
found that the Hausner ratio enabled one to distinguish
quantitatively between the free-flowing, easy-to-fluidise
group A and the cohesive, difficult-to-fluidise group C
powders. Essentially, it was found that cohesive group C
powders exhibited a ratio larger than 1.4 while powders
with a ratio less than 1.25 belonged to group A. Powders
with Hausner ratios in the range of 1.25 to 1.4 are in the
transitional group AC and have properties in common with
both A and C type powders. It must be stressed that
Hausner ratio reflects the friction conditions in a moing
w x
mass of powder rather than in a static situation 2 .
w x
Rastogi et al. 14 in studying dry ultrafine coals having
mean diameters of 7 to 25 mm, used Hausner ratios to
measure their cohesiveness. It was found that even with
over 1000 taps this ratio did not reach a steady state
indicating that further packing could be achieved. Using
Geldarts criteria of Hausner ratio as mentioned above,
they found that the Hausner ratio is consistent with other
parameters measured, such as floodability, deaeration in
fluidised bed and shear stress by the Jenike shear cell.
w x
Geldart et al. 13 , using irregular alumina, porous
cracking catalysts and fillites, and iron oxide, found that
the Hausner ratio was virtually independent of the relative
humidity of the air surrounding the particles even though
both the aerated and tapped bulk density varied as a
function of the relative humidity. However, Harnby et al.
w x
6 found the contrary. When working with different size
fractions of glass ballotini they observed a marked increase
in the Hausner ratio when a relative humidity of approxi-
mately 60% was exceeded for the 4553, 5363 and
6375 mm size fraction. This could be due to the non-por-
ous and smooth surface nature of ballotini where humidity
has no place to hide.
w x
Orband and Geldart 15 added antistatic agent, Laro-
stat
w
519, to three samples of pure terephthalic acid which
were known to have flow problems. With this antistatic
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 153
Fig. 1. The spherical shape of FCC particles.
agent the Hausner ratio of the most difficult powder was
lowered significantly from 1.66 to 1.27.
3. Materials used
Two types of powders were used in this work, in which
.
porous Fluid Cracking Catalyst FCC and non-porous Fire
.
Retardant Filler FRF grade powders mixtures were tested.
In each powder, a component of fine particles was added
to the coarse particles in weight percentages of 1, 2, 5, 10,
20, 40, 50, 60, 70, 80, 90 and 100%.
3.1. Fluid cracking catalyst
As the objective of this work was to study the effect of
particle size on the flowability of powder, the spherical
.
FCC see Fig. 1 used, which originally had a Sauter
diameter of 43.5 mm, was cut into two portions, i.e., fines
and coarse. The fines portion should, ideally, contain
particles with sizes less than 45 mm and the coarse portion
should be made up of particles larger than 45 mm. The
separation of this powder was performed in Hosokawa
Micron in Runcorn, Cheshire, on a Tumbler Screening
Machine ATS 600 with bouncing balls, which hit the
screen of a 61 mm sieve.
The coarse powder from this separation possessed all
the flow properties of a free-flowing powder, but the fines

portions flow properties i.e., the Hausner ratios1.16

.
and the angle of reposes29.28 differed little from the
coarse, so that it was not suitable to be used as cohesive
powder. A total of 30 kg of FCC was then sent to
Hosokawa Micron for grinding and this gave a fines
component with a mean Sauter diameter of about 7 mm
which behaved cohesively. The flow properties of these
two components of FCC is shown in Table 1.
3.2. Aluminium trihydroxide fire retardant fillers
.
Aluminium trihydroxide Fire Retardant Filler FRF is a
white crystalline powder with an angular particle shape
Table 1
Fines and coarse components of FCC powders
Fines FCC Coarse FCC
. Particle size, d mm 6.96 78.85
sv
Hausner ratio 1.78 1.12
3
. Aerated density kgrm 448 763
3
. Tapped density kgrm 797 853
a
. Angle of repose degree 43.9 27.3
Particle density 1242
. measured by gas flow method
3
. r kgrm
p
a
Angle of repose above 408 is considered cohesive.
.
see Fig. 2 and can be represented by the chemical
.
formula Al OH , alternatively written as Al O P3H O.
3 2 3 2
The non-porous FRFs are general purpose flame retardant
additives for use in a wide range of products based on
polyester, epoxy and acrylic resins, PVC, cellulosic materi-
w x
als and many elastomeric compounds 16 . FRF grade
powders have typical applications in glass reinforced plas-
tics and encapsulation resins. They are also used in exte-
rior cladding and tiles, synthetic marble, carpet and fabric
backing, conveyor belting, cables, furniture foam, PVC
and rubber goods, and adhesive, coatings and sealants.
FRF 5 and FRF 40 were chosen to be the coarse and
fine non-porous powders, respectively, in this study. The
Sauter diameters of these two powders are 63.1 and 6.6
mm, respectively, as measured by the dry method in the
Malvern Autosizer 2600C. As with FCC, the other proper-
ties of FRF 5 and FRF 40 were also tested before the fine
and coarse mixtures were made, to make sure that both did
behave as free-flowing and cohesive powders, respec-
tively. The results are shown in Table 2.
4. Experimental rig and procedure
4.1. Hosokawa Powder Tester
w x
Geldart and Wong 17 regarded the Powder Character-
istics Tester, type PT-D, designed by Hosokawa Mi-
Fig. 2. The angular shape of FRF particles.
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 154
Table 2
FRF 40 and FRF 5 Powders
FRF 40 FRF 5
. Particle size, d mm 6.6 63.1
sv
Hausner ratio 1.86 1.23
3
. Aerated density kgrm 654 1201
3
. Tapped density kgrm 1217 1480
a
. Angle of repose degree 54.4 29.1
Particle density 2449
. measured by gas flow method
3
. r kgrm
p
Helium Pycnometer 2447 2425
absolute density,
3
. r kgrm
abs
a
Angle of repose above 408 is considered cohesive.
.
cromeritics Laboratory Japan , as a very useful apparatus
for reproducibly measuring the physical characteristics of
powders. The incorporation of automation has eliminated
much of the human error typically present in such experi-
ments.
The aerated bulk density is measured by pouring pow-
der through a vibrating sieve into a cup. Fig. 3 shows the
equipment used, which is the assembly of a screen cover,
screen, a spacer ring, a chute attached to a mains-operated
vibrator of variable amplitude and a stationary chute aligned
w x
with the centre of a pre-weighed 100 ml cup 1 . A suitable
sieve, through which most of the material would pass
readily, has to be chosen. The combination of vibration
amplitude together with sieve aperture size should be such
that the time taken for the powder to fill the 100 cm
3
cup
is not less than 30 s. The excess powder is scraped from
the top of the cup using a ruler, without disturbing or
compacting the loosely settled powder.
.
For the tapped bulk density Fig. 3b , a cup extension
piece is fitted to the cup holding the aerated powder and
extra powder added into it, and then this whole setup is
subjected to tapping. A suitable number of taps needed to
be found. By performing a few tapped density measure-
ments at different number of taps, the number of taps
required for tapped bulk density to reach its maximum
could be determined. However, for this work a standard-
ised number of 180 taps over a period of 6 min, was used
in all cases. Care had to be taken during the tapping
process that the level of powder did not fall below the top
edge of the cup. When the tapping process finished, the
extension piece was removed and the powder then scraped
level with the top edge of the cup and the contents of the
cup weighed to obtain the tapped density. These experi-
ments were carried out at ambient conditions.
Five runs were conducted on each sample for aerated
density and tapped density. This leads to five independent
estimates for the Hausner ratio for each sample. The
average values were taken to be the aerated and tapped
bulk density, respectively.
4.2. Copley Tap Density Volumeter
Another tapping apparatus known as the Copley Tap
Density Volumeter was also used in order to see the effect
of a different tapping strength on the interparticle forces
within powders. The Copley volumeter consists of a gradu-
ated cylinder and tapping mechanism as shown in Fig. 4.
Fig. 3. The Hosokawa Powder Tester for measuring the aerated and tapped bulk densities.
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 155
Fig. 4. Copley Tap Density Volumeter.
The advantage of the Copley over the Hosokawa Tester is
that a fixed mass of powder is used, therefore there is no
need to remove the container for weighing as the number
of taps is progressively increased. The tapping action is
provided by a rotating cam driven by a 60 W motor with
an output speed of 250 rpm. The cam raises the cylinder
platform and hence the cylinder itself through a distance of
.
3 mm compared with 25 mm in the Hosokawa and then
drops again, therefore producing the tapping motion re-
quired. In this equipment, no specific method to measure
the aerated density is recommended by the manufacturer,
so the filling method used in the Hosokawa machine was
used.
About 100 ml of powder was first poured into the
graduated cylinder through the sieve from the Hosokawa
Powder Tester. Care has to be taken to switch off the
vibrating sieve when about 100 ml of powder have been
put into the volumeter. Normally, the powder does not
form a horizontal surface in the cylinder, therefore the
aerated density cannot be measured accurately, unlike the
Hosokawa Powder Tester, in which accurate volume and
powder weights are obtained when the powder is scraped
level before weighing. Later, this cylinder together with
the powder was put on the Copley volumeter with a rubber
sleeve around its base and subjected to the number of taps
desired. The tapped density is obtained by reading the
volume of the powder from the scale, but this is difficult
since the powder surface is seldom horizontal.
In order to overcome the problem of inaccurate volume
w x
3
reading Yusup 18 suggested using the 100 cm cup from
the Hosokawa tester on the base of the Copley. As in the
Hosokawa test, powder snowstorms into the 100 cm
3
cup
and after obtaining its aerated density, an extension piece
is placed on the cup and more powder is then added. The
cup with the extension piece together with the aerated
powder in it are then put on the Copley volumeter for
tapping. When the desired number of taps is reached, the
extension piece is then removed, the powder scraped level,
and the contents weighed to obtain the tapped density. For
the subsequent tapping, the extension piece is again placed
on the cup and more powder is added. This differs from
the use of the glass cylinder in which all powder experi-
ences same number of taps, whereas in the new technique
the recently added powder is only tapped for the subse-
quent number of taps, as done in the Hosokawa tester.
Using this modified technique, the tapped density can be
compared more meaningfully to the Hosokawa tapped
density as the error in reading the volume has been suffi-
ciently eliminated.
For convenience, the three methods used in tapping
have been named as:
Method 1: Hosokawa Powder Testers tapping as out-
lined in Section 4.1.
Method 2: Copley volumeters tapping where the gradu-
ated cylinder was used. This is named as Copley filling
and tapping in Figs. 1012.
Method 3: Hosokawas 100 cm
3
cup is filled by the
Hosokawa method and subjected to tapping in the Cop-
ley volumeter. This is called Hosokawa filling and
Copley tapping in Figs. 1012.
5. Results and discussion
It should be mentioned that all the results discussed in
Sections 5.1 and 5.2 were obtained using the Hosokawa
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 156
Fig. 5. Aerated density vs. mean particle size.
Powder Tester while in Section 5.3 both the Hosokawa
Powder Tester and the Copley Volumeter were used.
5.1. Hausner ratio, aerated and tapped densities
Figs. 5 and 6 show the aerated and tapped densities of
FRF and FCC mixtures. The densities of FRF grade mix-
tures are always higher than the FCC mixtures in both
aerated and tapped densities. The increase in particle size
initially increases the aerated and tapped densities of both
FRF and FCC mixtures. As particle size increases, the
cohesivity of powder is expected to decrease. A more
free-flowing powder should have a higher aerated density,
as the interparticle forces between particles become weaker,
therefore powder should pack in a denser condition. How-
ever, beyond the size of about 25 mm, further increase in
particle size shows no significant increase in the aerated
densities for both powder mixtures.
In the case of tapped density, initial increases in densi-
ties were followed by gradual decreases beyond a mean
particle size of about 15 mm for both powder mixtures.
However, the Hausner ratios of the two materials do not
vary very much from each other as shown in Fig. 7, where
the Hausner ratio decreases with the increase in particle
size. This confirms that the increase of particle size of a
powder mixture is always accompanied by the decrease in
cohesivity.
When powder mixtures are dominated by fine particles,
the interparticle forces, in this case the van der Waals
forces, should be dominant in the packing of particles
when they snowstorm down from the sieve into the 100
cm
3
cup. Due to this, low aerated densities are registered
when the particle size is small. The increase in particle size
slowly diminishes the influence of the van der Waals
force, thus causing the aerated density to increase. When
the van der Waals force becomes small or insignificant,
.
further increases in particle size beyond 25 mm do not
have much effect on the aerated density as shown in Fig.
5.
5.2. Duration of tapping
The tapped densities of both FRF and FCC mixtures
drop as more fines components are added to them as
shown in Fig. 6. This is particularly obvious with Sauter
Fig. 6. Tapped density vs. mean particle size.
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 157
Fig. 7. Hausner ration vs. Sauter diameter using tapped density measured after 180 taps.
diameter less than 15 mm for both mixtures. As mentioned
above, the interparticle forces are dominant due to the
presence of more fine particles. By using mechanical
force, i.e., tapping, it is expected that the density would
eventually reach a constant value as most of the mixtures
beyond mean size of 15 mm shown in Fig. 6. In order to
investigate the reason for the low tapped density observed
for mixtures less than 15 mm, three FRF powder mixtures
with large percentage of fines, i.e., 70, 80 and 90% of FRF
40, were chosen for further tapping beyond the 180 taps
used in the Hausner ratio test.
These three powder mixtures were subjected to a pro-
gressive increase in the number of taps up to a total of
1150 taps and their tapped densities resulting from these
high numbers of taps are as shown in Fig. 8. It should be
emphasised that in the process of increasing to higher
numbers of taps the same powder in the container is used
but with the more powder added. As experienced by
w x
Rastogi et al. 14 , after more than a thousand taps, all the
three mixtures still show no sign of attaining their respec-
tive constant densities. The tapped density increments due
to tapping from 180 to 1150 taps are rather small, i.e.,
6.0% for 70% FRF 40 mixture, 5.8% for 80% FRF 40
mixture and 7.3% for 90% FRF 40 mixture. This result
indicates that although a high number of taps was used,
i.e., the same repeated magnitude of mechanical force
applied, it is still not enough to overcome the interparticle
forces in the mixtures. The effect on the HR of increasing
from 180 to 1150 taps is shown in Fig. 9. The HR
increases by only about 5.8% for all the 70%, 80% and
90% FRF 40 mixtures in response to the increase of 970
taps for Method 1. The small increment in tapped density
and HR observed in a way justifies the use of a standard-
.
ised number 180 of taps used in all other measurements.
5.3. Comparison of Hosokawa with Copley tapping
In order to see if different tapping strengths could pack

the cohesive powder i.e., mixtures with more fine parti-

.
cles better, the Copley Tap Density Volumeter was used
Fig. 8. Tapped density vs. number of tapsMethod 1.
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 158
Fig. 9. Hausner ratio vs. Sauter diameter using tapped density measured after 180 and 1150 taps for 70, 80 and 90% FRF 40.
.
see Section 4.2 . This drops the powder only 3 mm
compared with 25 mm in the Hosokawa equipment.
Figs. 1012 show that the Hosokawa tapping gives
significantly higher densities than the other methods. In
both Methods 2 and 3, after 1150 taps the tapped densities
are still smaller than those of the 180 taps of Hosokawa
tester for all the three mixtures. This is almost certainly
because of the smaller dropping distance of the Copley

volumeter. In Methods 2 and 3 using the Copley volume-

.
ter , a constant value of the tapped density was reached
after 640, 740 and 760 taps for 70, 80 and 90% of FRF 40
mixture, respectively; 560, 540 and 520 for 70, 80 and
90% of FRF 40 mixture, respectively. Unlike the Hosokawa
.
tester Method 1 the tapped density continued to increase
slowly.
Methods 1 and 3 differ only in the manner in which the
powder is tapped. Both methods gave about the same
aerated density before tapping. After the initial 180 taps,
Method 1 registered tapped densities about 35% higher
than the tapped densities measured by Method 3. These
differences are reduced to about 19% at the end of 1150
taps. At this stage, tapped densities measured by Method 3
have already reached their respective constant values, but
tapped densities measured in Method 1 are still slowly
increasing, so the percentage difference could be higher if
the mixtures continue to be tapped. It is clear that the
Copley volumeter is unsuitable for assessing the flowabil-
ity of powders because the tapping provided cannot over-
come sufficiently the interparticle forces in cohesive pow-
ders.
Table 3 shows the aerated and tapped bulk densities as
well as the Hausner ratio for the three mixtures tested, in
the three different methods mentioned above. The tapped
densities shown are those obtained after 180 taps for all
the three mixtures. If the Hausner ratio of 1.4 is used as
the criteria in distinguishing cohesive and non-cohesive
powder, all the three mixtures were found to be cohesive
by Method 1 as shown in Table 3. However, the Hausner
ratios for all the three mixtures are less than 1.4 as
measured by Methods 2 and 3. It was obvious from
Fig. 10. Tapped densities for 70% FRF 40r30% FRF 5 obtained by three different methods.
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 159
Fig. 11. Tapped densities for 80% FRF 40r20% FRF 5 obtained by three different methods.
handling the three mixtures that they did possess strong
cohesivity, but the use of the tapped densities from the
.
Copley volumeter Methods 2 and 3 indicated incorrectly
that the mixtures were not cohesive.
Another interesting point in Figs. 1012, is that there is
always a crossover of tapped densities measured by Meth-
ods 2 and 3. At low numbers of taps Method 3 registered
higher tapped densities for all the three powder mixtures,
however at higher number of taps Method 2 would pack
the mixtures in a denser state. The crossover points are at
400, 580 and 600 number of taps for 70, 80 and 90% of
FRF 40 mixture, respectively. There may be three effects
at work here. In Method 3 because the steel 100 cm
3
cup
is filled by the Hosokawa technique, the aerated density is
already higher than in Method 2 which gives higher tapped
.
densities initially up to about 500 taps . Thereafter Method
2 leads to higher tapped densities because of the following.
.
a The different diameters of the container used, where
3
.
the 100 cm cup IDs5 cm is larger than the graduated
.
cylinder IDs3.5 cm . It is relatively easier to fill the
bigger diameter cup than the smaller graduated cylinder.
These are shown in the higher aerated densities recorded in
Method 3 compared to Method 2, where 10.0, 11.6 and
14.8% higher aerated densities are recorded for 70, 80 and
90% of FRF 40 mixture. As the mechanical force was
applied, the smaller diameter cylinder experienced a bigger
force per unit area so making the tapping energy more
concentrated per surface area. Although Method 3 started
with denser packing before tapping, as the number of taps
is increased the smaller diameter cylinder received a larger
cumulative force and eventually produced a denser pack-
ing. The lower number of taps in Method 3 required to
achieve constant densities for all the three mixtures also
.
implies that the lower force bigger diameter although
.
applied repeatedly higher number of taps could not over-
come the interparticle forces better than in the smaller
diameter cylinder Method 2.
.
b The Copley cylinder is glass which gives lower
powderrwall friction than the large steel container and
allows greater compaction.
Fig. 12. Tapped densities for 90% FRF 40r0% FRF 5 obtained by three different methods.
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 160
Table 3
Bulk densities measured by three different methods after 180 taps
Method Mixture Aerated Tapped Hausner
density density ratio
3 3
. . kgrm kgrm
70% FRF 40 808.1 1401.4 1.73
1 80% FRF 40 751.6 1338.0 1.78
90% FRF 40 691.9 1268.1 1.83
70% FRF 40 734.9 1006.7 1.37
2 80% FRF 40 673.6 910.3 1.35
90% FRF 40 602.7 861.0 1.43
70% FRF 40 800.4 1034.3 1.29
3 80% FRF 40 747.7 991.3 1.33
90% FRF 40 696.1 949.0 1.36
.
c In Method 2, the entire powder has been subjected
to the total number of taps whereas in Method 3, a
significant amount of powder has far fewer taps.
From this comparison of the results of these three
methods, the Copley volumeter is considered to be unsuit-
able for measuring the cohesivity of powder, due largely to
the weaker tapping strength built in to the apparatus.
Besides that, the other shortcomings of the Copley include
the absence of a standard filling method for the measure-
ment of aerated density and the inaccurate reading of the
volume of powder before and after tapping. However, the
Copley volumeter has the advantage of being mobile due
its smaller size and weight. The Hosokawa Powder tester
is a better apparatus as it has a good filling method,
reliable measurement and good built-in tapping mecha-
nism.
5.4. Effect of fewer fine particles in mixture
In Fig. 6, the increase in mean particle size has a great
influence on the arrangement of particles as they try to
form the densest packing. It should be remembered that a
large mean particle size corresponds to a small percentage
of the fine components. In a segregating system, when
powder is given mobility by tapping, the large and small
particles are able to rearrange to form the densest packing.
More large particles will provide more unoccupied voids
as most of the small particles would migrate to the bottom
of the cup to fill those voids in the lower region. This
would leave most of the voids in the middle and upper
region of the cup unoccupied.
.
In order to ascertain if tapping mechanical force does
give the freedom of movement to the fine particles to
reach to the bottom of the cup through the primary struc-
ture formed by the large particle, the tapped powders
compositions were checked. In this investigation, an FRF
mixture with 2% FRF 40 and 98% FRF 5 was used, as the
small percentage of fines available should make the segre-
gation phenomenon mentioned above easily observable if
it occurs. After the five measurements of aerated and
Table 4
Composition of 2% FRF 40 and 98% FRF 5 mixture after tapping
. . . Region Fines g Coarse g Total wt. g % Fines
Upper 6.11 24.64 30.75 19.9
Middle 6.08 25.32 31.40 19.4
Lower 5.97 25.38 31.35 19.0
tapped densities, the last tapped powder in the 100 cm
3
cup was divided into three regions, i.e., upper, middle and
lower, and about 30 g of samples were extracted from each
region. The compositions of fines in each region were
checked by separating fines from coarse using a 45 mm
sieve. The results are as shown in Table 4. A consistent
19% of fines -45 mm is observed in the three regions,
which firmly proves that it is not a segregating system.
Therefore, the reason for the lower tapped density
observed for mixtures with smaller percentage of fine
particles is simply that there are not enough fine particles
to fill the voids in between the large particles. It is
believed that the fine particles in these mixtures coated the
larger particles, and the repeated tapping simply could not
dislodge the fine particles from the larger particles. The
primary structure remains and there is no increase in
tapped density as no rearrangement of particles occurs.
Another FRF mixture with higher percentage of fine
particles, i.e., 20% FRF 40 and 80% FRF 5 mixture, was
also tested in the same manner, to check if the movement
of fine particles could be observed more clearly. The
results are shown in Table 5, where it is proven again that
a consistent percentage of fine particles is observed
throughout the three defined regions.
However, no test was carried out on the FCC mixtures,
as there were only limited amounts of fines and coarse
components of FCC available, and at the time this test was
performed most of the two components of FCC powders
were used up for fluidisation tests. Nevertheless, we are
quite sure that the same arguments used for explaining the
lower tapped density observed in FRF mixtures are also
valid for the FCC mixtures, as it has been proven convinc-
ingly in another test, using the Warren Spring-Bradford
Cohesion Tester, that the FCC mixtures are non-segregat-
ing systems.
5.5. Packing efficiency
Theoretically, it is possible to predict the maximum
density a packing could achieve. It is assumed that only
Table 5
Composition of 20% FRF 40 and 80% FRF 5 mixture after tapping
. . . Region Fine g Coarse g Total wt. g % Fines
Upper 11.85 24.78 36.63 32.4
Middle 11.46 24.18 35.64 32.2
Lower 10.78 23.73 34.51 31.2
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 161
Fig. 13. Voidage of aerated and tapped FRF mixtures.
the coarse particles, having a bulk density equal to their
tapped density, are in a container, and form a primary
structure. It is further assumed that when the fine particles
are mixed in they occupy the spaces between the large
particles at the same tapped density that they would have if
they were in a container on their own. If the initial volume
fraction of coarse and fine components, i.e., initial frac-

tional density of coarse and fine are, f and f 1y and

c f c
.
1y , and the particle density of the coarse and fine
f
components, r and r , are known, the maximum packing
c f
density can then be written as:
PD sf r q 1yf f r 3 . .
max c c c f f
where PD is the maximum packing density. The experi-
max
mental values of f and f are 0.61 and 0.5 for the coarse
c f
.
and fine FRF powders see Fig. 13 . The particle density
of fine and coarse components of FRF powder can be
.
found in Table 2. Inserting these values into Eq. 3 leads
to a value of PD of 1956 kgrm
3
compared with the
max
3
.
experimental value of 1650 kgrm see Fig. 6 , i.e., the
calculated value is 18.5% higher.
The experimental values of f and f for FCC are 0.60
c f
.
and 0.56 Fig. 14 , respectively. The gas flow technique,
as outlined in the Appendix A, was used to measure the
particle density for the porous FCC, but because of effects
such as channelling this method could not be used to
measure the particle density of the fines component of
FCC and there is no other known method to do this. Since
it was impossible to measure the particle density of the
fine FCC, and because it is known that at maximum
.
packing density Fig. 16 there is always more coarse
material than fines, the particle density of FCC fines was
taken to be the same as that of the coarse FCC, i.e., of
3
.
1242 kgrm . By substituting these values into Eq. 3 , the
calculated PD of FCC is 1023 kgrm
3
, which is very
max
close to the experimental value of 1040 kgrm
3
.
The reason for the closer match between the calculated
and the experimental value of PD for FCC compared to
max
that for FRF powder could be due to the shape difference
Fig. 14. Voidage of aerated and tapped FCC mixtures.
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 162
Fig. 15. Density vs. percentage of FRF 40 in mixture.
of these two powders. The fines component of the FCC
particles could roll in between the larger spherical particles
.
see Fig. 1 thereby forming a dense packing which almost
equals the theoretical estimation. However, the more angu-
.
lar fine FRF particles see Fig. 2 might not be able to roll
and find their way as easily as the FCC, therefore leaving
more voids in between the larger particles, and contribut-
ing to an experimental PD lower than the theoretical
max
estimation.
5.6. Voidage profile
Figs. 13 and 14 show the voidage of aerated and tapped
powders for both mixtures. The voidage of aerated powder
initially decreases with the increase in particle size and
later stays virtually constant. However, the voidage for the
tapped powder initially decreases, and after reaching its
minimum values, increases again which is what was men-
tioned above as there are not enough small particles to fill
the voids in between the larger particles. These effects are
observed in both powder mixtures.
In order to calculate bed voidages, it is essential to
.
know the envelope or apparent density of the particles.
This is also known as the particle density and is defined as
the mass of the particle divided by its volume, where this
density is different from absolute or skeletal density if the
particle is porous, since the volume in question contains all
w x
pores, open or closed. It has been shown by Xie 19 that
coarse FCC particles have a lower particle density than the
fines. As we were unable to measure r for the fines in
p
order to calculate the r for the mixtures, r for the as
p p
.
received FCC which contained a wide range of sizes
.
was measured by the gas flow technique see Appendix A
and found to be 1418 kgrm
3
. This value has been used to
calculate the voidage shown in Fig. 14. For the non-porous
FRF mixtures, r was obtained using the helium pyc-
p
nometer.
5.7. Critical size
w x w x w x
Grey and Beddow 2 , Wong 20 and Orband 21
observed that Hausner ratios increase with the decrease of
Fig. 16. Density vs. percentage of fines FCC in mixture.
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 163
w x
particle size. Orband 21 discovered that there is a critical
size above which Hausner ratio is virtually constant, which
means to say that powders do not possess any cohesivity;
it is only below this critical size that the Hausner ratio
increases with the decrease of particle size. However, from
the data of FRF and FCC mixtures as shown in Fig. 7, a
critical size for either mixture cannot be categorically
determined. Instead the Hausner ratios for both mixtures
are proportional to 1rd
0.2
. If a critical size exists, then it is

believed that it should fall in range of 1.25-1.4 range

.
represented by two dotted lines in Fig. 7 , which is also
known as Geldarts group AC powder. The corresponding
particle size in this region for FCC is 25-d -42 mm,
sv
where below this size range Hausner ratios increase with
the decrease of particle size; and above this size range
interparticle forces, especially the van der Waals forces,
become less influential in the packing of powder. For the
FRF mixture, the critical size is in the range of 30-d -
sv
54 mm.
5.8. The packing of powder
Although the particles used in this work do not have the
same shape and are made up of the two different mean
sizes mentioned earlier, they somehow do show a similar
pattern of density change to each other with the increase in
percentage of smaller particles. Figs. 15 and 16 show that
.
the tapped densities random dense packing of both pow-
ders change in the same manner as in Fig. 17, which is the
basic behaviour of random dense packing of binary mix-
w x
tures of spherical particles sketched by Furnas 22 .
The tapped density curves for both powders also con-
firmed that maximum densities for mixtures are achieved
with more large particles in the mixture, as stated by
w x
Furnas 22 . For the FCC mixtures the maximum tapped
density is achieved with about 38% of fines in the mixture.
This matches closely the 35% of fines in mixtures pre-
Fig. 17. The packing density variation with composition for a bimodal
mixture. The maximum density for a homogeneous mixture f
)
occurs at
a composition X
)
. Two-dimensional structures are shown for five possi-
w x. ble compositions after German 25 .
Fig. 18. The porosity vs. composition for bimodal mixtures of varying
particles size ratios, assuming an inherent fractional packing density of
w x. 0.5 after Furnas 22 .
w x
dicted by Furnas 23 for particle size ratios about 10:1 as
shown in Fig. 18. This could mean that the many models
developed for the prediction of packing of binary mixtures
could also be applied to powders with distribution of sizes.
The fines percentage which gives maximum tapped density
.
in FRF mixtures is less clearly seen Fig. 15 but is in the
range of 2040%.
5.9. Effect of particle size ratio and shape
The particle size ratio based on the Sauter mean diame-
ters for FRF and FCC mixtures are 9.6:1 and 11.3:1,
respectively. The minimum voidage of the tapped FCC
mixtures is 0.27 at a mean particle size of 15 mm, and for
the FRF mixtures is 0.32 at a mean particle size of about
23 mm. Despite the relatively small difference in the
particle size ratio in this two mixtures, the bigger size ratio
mixture still proved to have packed better, which is in line
w x
with that shown in Fig. 18 as stated by Furnas 22 .
The more significant difference between these two pow-
ders is their shape. The FCC particles are more spherical
.
Fig. 1 whereas the FRF particles are more angular Fig.
.
2 . The reason why FCC mixtures packed better than FRF
mixtures is influenced more by the shape of the particle
rather than the small particle size ratio difference. This
w x
result agreed with that found by Yerazunis et al. 24
where the spherical glass mixtures they used showed better
packing in comparison with the non-spherical glass mix-
.
tures crushed which have about the same particle size
ratio.
6. Conclusions
Although the FRF grade and FCC mixtures are not
perfectly spherical particles, they both exhibit density pat-
terns similar to those of an assembly of bimodal spherical
particles. The maximum packing density always occurs
when there is a smaller mass fraction of fine particles in a
mixture compared to larger particles. The maximum pack-
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 164
ing densities for the FRF and FCC mixtures are observed
at 2040% FRF 40 and about 38% fine FCC, respectively.
These values are similar to those mentioned by Furnas
w x
23 . The particle shape does play a role in making denser
packing. The more spherical shaped FCC mixtures packed
better than the more angular shaped FRF mixtures.
It is well known that the cohesivity of powder decreases
with the increase in particle size, and this was confirmed
for both powder mixtures by means of the Hausner ratio. A
critical mean size above which the increase in mean
particle size would see no significant effect on the cohesiv-
ity of the powder cannot be categorically seen from the
data of the FRF and FCC mixtures. However, below a
value of HR less than 1.25, interparticle forces become
less significant with the increase of particle size; above the
.
HR range for group AC powders 1.251.4 , cohesivity
increases rapidly with the decrease of particle size.
There is evidence that in both FRF and FCC mixtures,
when fine components are added to the coarse particles
they adhere strongly to the large particles, preventing
percolation of fines to the bottom of the mixtures.
The Hosokawa Powder Tester when used to charac-
terise flowability gives more reliable measurements than
the Copley Volumeter, as accurate powder weights can be
measured.
7. Symbols and abbreviations
..
b a constant Eq. 2
d Sauter diameter
sv
f , f fractional density of coarse or fine particle
c f
fraction
FCC Fluid Cracking Catalyst
FRF Fire Retardant Fillers
HR Hausner ratio
K constant of CarmanKozeny equation
L, L , L bed height, at aerated state and tapped state,
A T
n number of taps
PD the maximum packing density
max
S , S slope of plot DP vs. U for aerated and tapped
A T
..
T compaction constant Eq. 1
U superficial velocity or empty tube velocity
S r
A BT
.
y s P
S r
T BA
c sphericity of particle
r , r bulk aerated or tapped densities
BA BT
r tapped density after n taps
n
r particle density
p
r maximum tapped density
`
r , r particle density of coarse or fine particles
c f
D p pressure drop
m viscosity of gas used in fluidisation
, , voidage in aerated state and tapped state,
A T
respectively
Appendix A
An easy way to measure particle density of a porous
powder is the gas flow technique, which is based on the
Erguns equation. This technique is suitable for powders
that have a significant difference between their aerated and
tapped densities. As this method depends greatly on mea-
suring the pressure drop across a fixed bed, it is not
suitable for cohesive powders in which channelling is
likely to occur.
The primary task of this technique is to measure the
pressure drop and bulk density of the bed at two voidages,
i.e., the aerated and tapped beds. In the aerated state, the
bed should be in its loosest form where it attains maximum
voidage. The method to achieve this is by first fluidising
the powder to mix it well and then let it settle by itself.
The bed height at the aerated state is designated as L , and
A
pressure drop, D p, is measured for at least four superficial
gas velocities. After that the bed is tapped to allow the
powder bed to achieve a much lower voidage. The new
bed height in the tapped state is designated as L , and
T
again D p is measured. The plot of DP against the superfi-
cial velocity for both the aerated and tapped bed give two
slopes S and S , respectively. By referring to the Ergun
A T
equation, the first term on the right-hand side of that
equation which is called the CarmanKozeny equation can
be written as:
2
Dp K 1y mU .
s P . A1 .
3 2
L d
sv
.
By rearranging the Eq. A1 and putting subscript A for
the aerated experiment, the slope of the graph can be
written as:
2
DP Km 1y .
A
S s s L . A2 .
A A 2 3
/
U d
A sv A
Similarly, the slope for tapped bed can be written as:
2
DP Km 1y .
T
S s s L . A3 .
T T 2 3
/
U d
T sv T
It is known that
L r
A BT
s A4 .
L r
T BA
and
r
BA
1y s A5 .
A
r
p
r
BT
1y s A6 .
T
r
p
( ) E.C. Abdullah, D. Geldart rPowder Technology 102 1999 151165 165
where r and r are the bulk densities for aerated and
BA BT
. .
tapped beds, respectively. Dividing Eq. A5 by Eq. A6
and substituting for L , L , and
A T A T
S r r yr
A BA p BT
s . A7 .
S r r yr
T BT p BA
S r
A BT
By assigning ys P A8 .
/
S r
T BA
particle density can be written as:
r yy
1r3
Pr
BT BA
r s . A9 .
p 1r3
1yy
The most important point in using this method is to
measure accurately the pressure drop across a fixed bed.
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