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The influence of particle size distribution and tapping on the bulk density of
milled lactose powders

Conference Paper · September 2013

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 The Influence of Particle Size Distribution and
Tapping on the Bulk Density of Milled Lactose
Powders
Horng Yuan Saw1,2, Clive E. Davies1,2, Anthony H.J. Paterson1 and Jim R. Jones1
1
School of Engineering and Advanced Technology
Massey University, Palmerston North 4442, New Zealand
Email: H.Y.Saw@massey.ac.nz
2
Riddet Institute, Massey University, Palmerston North 4442, New Zealand
Email: C.Davies@massey.ac.nz

Abstract— When an external force is applied to a bed of
loosely packed powder via tapping, the particles in the bed
rearrange themselves and fill up the inter-particle voids,
resulting in higher packing density. The rearrangement of
particles is dependent on size distribution, level of fines,
magnitude of inter-particle forces, and operating
parameters like number of taps and powder bed drop
height. In this study, we report the tapped density, ρtap, of
thirteen milled lactose powders obtained with a tapping
apparatus (3 mm drop height, ~240 strokes min–1) in the
range of 10–1250 taps, in accordance with the European
Pharmacopeia. The ρtap profiles can be modelled with the
Kawakita powder compression equation, [(ρtap–
ρ0)/ρtap]=[atbtN/(1+btN)], where ρ0 is the initial bulk
density, N is the number of taps, and at and bt are fitting
parameters that reflect the compression characteristics of
the powder. Our at and bt data are consistent with
literature values for lactose powders; at relates well with
particle size but bt data show significant scatter. On a
heuristic basis, parameter at is further correlated with
surface-volume mean particle diameter, d*32, span of the
particle size distribution, (d90–d10)/d50, and the fraction of
fines less than 45 μm, F45. A power law relationship in the
form of at=m([1/d*32][(d90–d10)/d50][exp(F45)])n is found; the
product ([1/d*32][(d90–d10)/d50][exp(F45)]) accounts for the
combined influence of particle size distribution on powder
compressibility. Our findings are potentially useful in the
handling and packaging of food and pharmaceutical
materials.
Keywords- bulk density; Kawakita equation; lactose;
particle size distribution; powder compression; tapped
density
I. INTRODUCTION
Bulk density is an important physical property in the
characterization, handling, and processing of powder systems.
It is the mass divided by the total volume occupied, taking into
account the inter-particle and intra-particle voids in a bed of
powder. There are two common bulk densities, namely loose
poured bulk density, ρLB, and tapped bulk density, ρtap. Loose
poured bulk density is the density of a powder that is poured
into a container and allowed to settle gently; it is a measure of
random loose packing. Tapped density is the density obtained
after a loosely packed powder bed is densified with an
external force to achieve higher particle packing; it is a
measure of random dense packing, see the review in [1,2]. The
ratio ρtap/ρLB is known as Hausner ratio, HR [3], and it is
commonly used as a crude powder flow descriptor; see for
example [1].
The bulk density of a powder is dependent on its particle
size distribution. It has been experimentally demonstrated that
both ρLB and ρtap relate well with surface-volume mean particle
diameter, d32, and the content of fines; HR increases when d32
decreases and fines level increases [1]. As d32 decreases, the
powder becomes more cohesive and occupies more volume in
the loosely poured state than free flowing particles; they have
greater interparticle forces and internal bed strength to
maintain bed structure. But when an external force is
introduced to the cohesive powder bed, the interparticle forces
are overcome and the volume reduces significantly, hence
giving higher HR values.
In this paper, we report the influence of particle size, span
of the particle size distribution, and fines level on the bulk
density of fine lactose powders, which have wide applications
in the food and pharmaceutical industries. A tapping apparatus
with a 3 mm drop height and ~240 strokes min–1 tapping rate
was used; following the European Pharmacopeia the number
of taps was up to 1250 taps [4]. This work forms part of a
wider study in which the physical and flow properties of fine
powders are characterized. The findings here can potentially
benefit the food and pharmaceutical industries in areas like
powder compression and packaging of fine materials.
 II. EXPERIMENTAL III. ANALYSIS
In the first part of this work, the relationships between d*32
A. Sample Preparation
and (d90–d10)/d50, and between d*32 and F45 were evaluated;
A total of 13 model milled lactose powders were used, and d*32 was plotted against (d90–d10)/d50, and 1/d*32 was plotted
each powder was designated a code, see Table 1. Three against F45.
powders, which were commercial lactose of DMV-Fonterra
Excipients, New Zealand, were used as received (unsieved), In the second part, the Kawakita model [8], Equation 1,
namely lactose monohydrate Pharmatose® 70M (LP1), was used to assess tapped density as a function of number of
Pharmatose® 350M (LP4), and Hydrous Refined Lactose 100- taps; N is number of taps, mtap is sample mass after Nth tap, m0
Mesh (LM1). The other ten powders were made by sieving is sample mass in the loose poured state, and at and bt are
either LP1 or LM1; further details are available in [5]. fitting parameters that reflect the characteristics of the powder.
Rearranging Equation 1, and taking into account a constant
B. Measurement of Particle Size Distribution volume tapping system, Equation 2 was obtained; the values
Particle size distribution was measured on the volume- of at and bt were obtained by linear regression.
weighted basis by the laser diffraction method (Mastersizer
ρ tap − ρ0 at bt N
2000, Malvern Instruments Ltd., UK); the 300 RF lens and = (1)
small volume sample unit with isopropanol as the dispersant ρ tap 1 + bt N
were used. The refractive index of lactose (1.533) and
isopropanol (1.378), and the default Polydisperse model were mtap N 1 1
= N+ (2)
selected. Table 1 lists the size distributions; diameters d10, d50, mtap − m0 at at bt
and d90 represent particle size at 10%, 50%, and 90% in a
cumulative size distribution respectively. The span of a size
distribution is given by (d90–d10)/d50. Parameter d*32 is the Lastly, the relationships between parameters at and bt and
surface-volume mean diameter calculated with the Mastersizer particle size distribution were investigated; both at and bt were
data using bins equivalent to a full sieve analysis according to respectively plotted against d50, 1/d*32, and the product
BS 410; powder in the range 0–38 μm was grouped together ([1/d*32][(d90–d10)/d50][exp(F45)]).
and assigned a mean diameter 19 μm, see [5]. Parameter F45 is
the fraction of fines smaller than 45 μm.
IV. RESULTS
C. Measurement of Loose Poured and Tapped Densities Table 1 shows the particle size distribution, d*32, and fines
level of the milled lactose powders.
Loose poured bulk density, ρLB, was measured following a
modified New Zealand standard [6]. About 400–500 g of
material were poured vertically into a 500 ml cylindrical TABLE I. PARTICLE SIZE DISTRIBUTION, SURFACE-VOLUME MEAN
PARTICLE DIAMETER, AND FINES LEVEL OF MILLED LACTOSE POWDERS
container through a cone (46.6o internal angle; 12.7 mm
orifice diameter); the distance between the cone outlet and Lactose Particle diameter [μm] Level of
container brim was ~70 mm. In cases where the powder did d10 d50 d90 d*32 fines <45
μm, F45 [-]
not flow through the cone, manual stirring with an art brush
was applied. Excess powder on the container was gently LP4 7.3 34.5 85.3 28.9 0.585
scraped off with a steel ruler, and the filled container was LM7 7.1 37.4 81.6 29.9 0.551
LM8 9.0 56.1 110.2 39.3 0.355
weighed. Measurements were done in triplicate; the mean LM9 10.2 64.4 125.3 43.3 0.304
values were calculated. LM1 14.4 108.5 256.2 58.0 0.221
LM4 16.1 139.5 239.7 65.1 0.195
Tapped density, ρtap, measurements were based on a LM2 26.9 112.9 190.8 73.4 0.121
method for dry dairy products [7] and the European LP2 36.4 139.0 232.3 83.6 0.110
Pharmacopeia [4]. A Stampfvolumeter tapping machine LM3 81.8 143.2 219.2 110.7 0.047
(STAV 2003, Engelmann, Germany) with a 3 mm drop height LM5 40.5 251.8 403.7 113.4 0.102
and a tapping rate of ~240 taps min–1 was used. The machine LP1 88.6 257.0 538.4 150.8 0.050
LM6 141.7 242.0 386.5 163.7 0.045
comprised a 100 ml cylindrical cup of 42.05 mm internal
LP3 178.2 263.4 373.0 223.0 0.018
diameter, which was extendable by 35 mm in height with a
stainless steel extension. For very fine lactose powders, a
cylindrical cardboard tube of a similar diameter and 100 mm Figure 1 shows d*32 plotted against span (d90–d10)/d50; the
in height was needed and attached to increase the powder mean particle diameter increases with decreasing span. There
mass. The number of taps used was 10, 35, 100, 180, 500, are also irregularities in the plot; the sieved powders deviate
1000, and 1250. At each increment, the extension was from the trends exhibited by the powders that are used as
removed carefully and excess material on the 100 ml cup was received. In Figure 2, the reciprocal of d*32 is plotted against
gently scraped off with a steel ruler; the amount of material in F45; as expected mean particle diameter decreases as fines level
the cup was then weighed. Repeat measurements were made increases. The data for unsieved and sieved powders seems to
fall on one line.
on selected samples and the results were reproducible.
 Figure 4 shows the relationship between parameter at and
d50, and in Figure 5 the relationship between parameter bt and
d50; for comparison purposes some data from the literature
[9,10] are included. Parameter d50 is used because d*32 values
are not reported in the work cited. By inspection of Figure 4, at
generally increases with decreasing d50; our data are consistent
with the milled lactose data by Soh et al. [9] and Ilić et al. [10].
However, agglomerated and spray-dried lactose powders seem
to show different trends. Referring to Figure 5, the milled
lactose data are scattered and there is difficulty in defining
clear trends. And consistent with Figure 4, the agglomerated
and spray-dried lactose powders seem to exhibit trends
different from the milled lactose.

Figure 1. Plot of d*32 versus span (d90–d10)/d50.

Figure 4. Plot of parameter at versus d50 for lactose powders.

Figure 2. Plot of 1/d*32 versus F45.

Figure 5. Plot of parameter bt versus d50 for lactose powders.

Figure 6 shows at increasing almost linearly with 1/d*32 for

both unsieved and sieved lactose powders. In Figure 7, the bt
data are scattered, but seem to increase to a peak and then
Figure 3. Plot of ρtap versus N for lactose LP4 and LP3. decrease. In Figure 8, at is plotted against ([1/d*32][(d90–
d10)/d50][exp(F45)]) and a power law relationship is observed
Figure 3 shows the tapped density profiles of lactose LP4 for both unsieved and sieved lactose powders, giving Equation
and LP3, plotted to illustrate the significance in density 3 with an R2 of 0.96.
changes when powder cohesiveness increases. For free flowing
LP3, the change in ρtap is relatively small with increasing taps.  1  d − d  0.376
But with LP4, which is the most cohesive sample used, ρtap at = 0.00536  90 10
 exp(F45 ) (3)
 d 32  d50 
*
increases significantly from ~530 to ~780 kg m–3. 

Figure 6. Plot of parameter at versus 1/d*32.
Figure 7. Plot of parameter bt versus 1/d*32.
Figure 8. Plot of parameter at versus ([1/d*32][(d90–d10)/d50][exp(F45)]).
V. DISCUSSION
There are three ways to densify a bed of powder, viz
tapping, vibration, and mechanical compression; in this work
only tapping was used. During tapping, powder densification
happens in an unconfined condition; the particles are forced to
‘jump’ and lose contacts with adjacent particles. Due to the
relative particle motion, the particles rearrange themselves and
fill up the voids in the powder bed, resulting in higher particle
packing [1,2]. We have assumed that no particle deformation
occurs to the crystalline lactose particles.
The relationship between ρtap and N can be modelled;
many empirical mathematical expressions are available, see
for example the list compiled by Kawakita and Lüdde [8], and
their use is common and convenient. We have chosen the
Kawakita equation because of its applicability with different
powders and low number of taps, as demonstrated by others
[9–12]. The model is simple and contains only two fitting
parameters, at and bt. However, though any physical
significance is unclear we have examined our data for
correlation between these fitting parameters and the physical
properties of the test powders.
The parameter at for various types of powders has been
reported to increase with decreasing particle size [8,11]; the
lactose data in Figure 4 show a similar trend. The data in the
figure also suggest that the at:d50 relationship is material
specific; agglomerated and spray-dried lactose powders do not
seem to follow the milled lactose trend. The reason can be
attributed to the differences in particle shape, asperities, and
moisture content, which are factors that can affect particle
packing. Microscopic images and more experimental data are
required to make further deductions. Referring to Figure 6,
parameter at correlates well with the reciprocal of d*32, which
is a measure of the ratio of particle surface area to volume;
1/d*32 has been used previously in a correlation that relates the
cohesion of compacted powder beds to surface area per unit
volume and compaction forces [5].
According to Yamashiro et al. [11], parameter bt generally
increases with increasing particle size; when their data are
plotted, scatter and discontinuities are observed because their
powders, e.g. glass beads, calcium carbonate, iron powders,
and talcum, are very different in their physical properties.
Referring to Figure 5, scatter and discontinuities are also seen
with lactose powders, possibly because of the unaccounted
differences in other physical properties besides particle size. In
Figure 7, bt seems to peak at a value of 1/d*32 of about 20,000
m–1; we are also not able to explain the apparent increasing
and decreasing trend.
Parameter at represents the asymptotic value of [(ρtap–
ρ0)/ρtap] when N approaches infinity and equals [1–(1/HR)]; see
[12,13]. Yu and Hall [12] related at and bt empirically to a
limiting Hausner ratio – the ratio at very high number of taps,
HR,∞ achieved with manual tapping – and proposed Equations
4 and 5 for alumina and silicon carbide powders. A similar
approach but using Hausner ratio at 1250 taps, HR,1250, gives
Equation 6 with an R2 of 0.99; thus at is equal to [1–
(1/HR,1250)] for the milled lactose powders.
No satisfactory correlation is found for bt; it is numerically
small compared to at and is consistent with the limit of
Equation 1 as bt approaches zero. Averaging the bt data gives a
value of 0.0447 with a standard deviation of 0.0134.
  1.092
1 
at = 1.4351 −  (4)
 H R,∞ 
−1.762H R,∞
bt = 6.244 ×10 (5)
1.003
 1 
at = 1.0111 −  (6)
 H R,1250 
To date, there is no conclusive report in the literature on
how parameters at and bt relate to the key descriptors of a
particle size distribution, namely d*32, (d90–d10)/d50, and fines
content F45 for example, which also influence each other, see
Figures 1 and 2. On a heuristic basis and as shown in Figure 8,
at relates satisfactorily with the function ([1/d*32][(d90–
d10)/d50][exp(F45)]), which can represent the influence of a size
distribution. The term exp(F45) is also found in correlations for
the characterization of bed collapse phenomena in fluidized
beds [14].
CONCLUSIONS
Thirteen milled lactose powders were densified via tapping
following the European Pharmacopeia procedure and the
changes in bulk density were characterized with the Kawakita
equation that comprised fitting parameters at and bt. The
parameters showed initial trends relating to particle size, and
further attempts were taken to correlate them with 1/d*32, (d90–
d10)/d50, and F45. Parameter at was observed to be a function of
([1/d*32][(d90–d10)/d50][exp(F45)]) and related well to Hausner
ratio at 1250 taps. Parameter bt was numerically small and no
conclusive correlation with material properties was identified.
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