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Pharmaceutical
Physics
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Particle-Size Distribution, Part I

Representations of Particle
Shape, Size, and Distribution
Harry G. Brittain

I
Particle-size determinations are undertaken
to obtain information about the size
characteristics of an ensemble of particles.
Because the particles being studied are not
usually the exact same size, information is
required regarding the average particle size
and the distribution of sizes about this
average. However, the concept of particle
size is irrevocably derived from aspects of
particle shape and morphology because the
idea of a particle diameter proceeds from
preconceived shape factors.

n the July 2001 Pharmaceutical Technology article about

particle-size determination, the question of what constitutes
a correct method for the determination of particle-size distributions was addressed (1). A correct method was defined as
one whose sample was obtained by an appropriate sampling procedure, in which the sample was prepared properly and introduced into the instrument, and in which all instrumental parameters were used correctly for the analysis. It also was pointed
out that all of the correct (but differing) particle-size results obtained through various methodologies are equally accurate, but
each method simply might be expressing its correct results in
different terms. When viewed in this light, the decision about
which particle-size methodology is most appropriate for a given
situation can be seen as a simple matter of accuracy versus precision. If absolute accuracy is most important, then one must
conduct rigorous research to verify that the method finally
adopted does indeed yield particle-size results that are absolutely
indicative of the characteristics of the bulk material. If, however,
one is more interested in developing profiles of lot-to-lot variability, then the use of any of the available methods that yields
correct results is appropriate.
The next several articles in the Pharmaceutical Physics column series will examine a variety of correct methodologies that
can be used to deduce information about the shape and size
distribution of particles. However, one cannot begin to address
those topics without a prior exposition of what is meant by the
shape and size of the particles that consitute a powdered solid.

Particle shape

Harry G. Brittain, PhD, is the director of

the Center for Pharmaceutical Physics, 10
Charles Road, Milford, NJ 08848, tel. 908.
996.3509, fax 908.996.3560, hbrittain@
earthlink.net. He is a member of Pharmaceutical Technologys Editorial Advisory
Board.

38

Pharmaceutical Technology

DECEMBER 2001

It is not possible to discuss rationally the size of a particle or

any distribution associated with the sizes of an ensemble of particles without first considering the three-dimensional characteristics of the particle itself. This is because the size of a particle is expressed either in terms of linear dimension characteristics
derived from its shape or in terms of its projected surface or
volume. As will be shown, some methods of expressing particle size discard any concept of particle shape and instead express the size in terms of some type of equivalent spherical size.
An appropriate starting place for a discussion of particle shape
can be found in USP General Test ^776& (see Figure 1) (2). In the
shape performance aspect of this particular test procedure, USP
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requires that for irregularly shaped particles, characterization

of particle size must also include information on particle shape.
The general method defines several descriptors of particle shape
(see Figure 2). The USP definitions of these shape parameters are
acicular: slender, needle-like particle of similar width and
thickness
columnar: long, thin particle with a width and thickness that
are greater than those of an acicular particle
flake: thin, flat particle of similar length and width

Plate

Tabular

Equant

Columnar

Blade

Acicular

Figure 1: Description of particle shape as defined by USP.

Lamellar

plate: flat particle of similar length and width but with greater
thickness than flakes
lath: long, thin, blade-like particle
equant: particles of similar length, width, and thickness; both
cubical and spherical particles are included.
In ordinary practice, one rarely observes discrete particles but
typically is confronted with particles that have aggregated or agglomerated into more-complex structures. USP provides several terms that describe any degree of association:
lamellar: stacked plates
aggregate: mass of adhered particles
agglomerate: fused or cemented particles
conglomerate: mixture of two or more types of particles
spherulite: radial cluster
drusy: particle covered with tiny particles (2).
The particle condition also can be described by another series of terms:
edges: angular, rounded, smooth, sharp, fractured
optical: color, transparent, translucent, opaque
defects: occlusions, inclusions.
Furthermore, surface characteristics can be described as
cracked: partial split, break, or fissure
smooth: free of irregularities, roughness, or projections
porous: having openings or passageways
rough: bumpy, uneven, not smooth
pitted: small indentations.
The pharmaceutical descriptors of particle shape are derived
from the general concept of crystallographic habit. The exact
shape acquired by a crystal will depend on various factors such
as the temperature, pressure, and composition of the crystallizing solution. Nevertheless, precipitation of a given compound
generally creates a characteristic shape or outline. Because the
faces of a crystal must reflect the internal structure of the solid,

Tabular

Equant

Columnar

Acicular

Isometric
Tetragonal

0001
Hexagonal

1011

0111

Figure 2: Growth along certain crystal directions can profoundly alter the characteristic habit of various crystals.
40

Pharmaceutical Technology

DECEMBER 2001

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(a)

(b)

(c)
Feret's diameter

th

ng

Le

Martin's
diameter

Projected
area
diameter

idt
h

Figure 3: Some commonly used descriptors of particle size.

the angles between any two faces of a crystal will remain the
same even if the crystal growth is accelerated or retarded in one
direction or another (see Figure 2). Optical crystallographers
usually will catalogue the various crystal faces and document
the angles between them as they identify the crystal system to
which the given particle belongs. When the particle is particularly well formed, a description of symmetry elements also is
compiled.
For many individuals, however, the concept of qualitative
shape descriptors has proven inadequate, and this deficiency
has necessitated the definition of more quantitatively defined
shape coefficients (3). For instance, Heywood describes the elongation ratio, n, as
[1]
and the flakiness ratio, m, as
[2]
in which T is the particle thickness (the minimum distance between two parallel planes that are tangential to opposite surfaces
of the particle), B is the breadth of the particle (the minimum
distance between two parallel planes that are perpendicular to
the planes defining the thickness), and L is the particle length
(the distance between two parallel planes that are perpendicular to the planes defining thickness and breadth) (4).

Particle size
It really is not possible to continue a discussion of particle shape
or size without first developing definitions of particle diameter. This step is, of course, rather trivial for a spherical particle
because its size is uniquely determined by its diameter. For irregular particles, however, the concept of size requires definition by one or more parameters. It often is most convenient to
discuss particle size in terms of derived diameters such as a
spherical diameter that is in some way equivalent to some size
property of the particle. These latter properties are calculated
by measuring a size-dependent property of the particle and relating it to a linear dimension.
Certainly the most commonly used measurements of particle sizes are the length (the longest dimension from edge to edge
of a particle oriented parallel to the ocular scale) and the width
(the longest dimension of the particle measured at right angles
to the length). Intuitive as these properties may be, their definition still is best shown in Figure 3a. Closely related to these properties are two other descriptors of particle size: Ferets diameter,
42

Pharmaceutical Technology

DECEMBER 2001

which is the distance between imaginary parallel lines tangent to a randomly oriented particle and perpendicular to
the ocular scale, and Martins diameter, which is the diameter of the particle at the point that divides a randomly oriented particle into two equal projected areas (see Figure
3b).
The coordinate system associated with the measurement
is implicit in the definitions of length, width, Ferets diameter, and Martins diameter because the magnitude of
these quantities requires some reference point. As such,
these descriptors are most useful when discussing particle size
as measured by microscopy because the particles are immobile.
Defining spatial descriptors for freely tumbling particles is considerably more difficult and hence requires the definition of a
series of derived particle descriptors. However, given the popularity of techniques such as electrozone sensing or laser light
scattering, derived statements of particle diameter are extremely
useful.
All of the derived descriptors for particle size begin with the
homogenization of the length and width descriptors into either
a circular or spherical equivalent and make use of the ordinary
geometrical equations associated with the derived equivalent.
For instance, the perimeter diameter is defined as the diameter
of a circle having the same perimeter as the projected outline of
the particle. The surface diameter is the diameter of a sphere having the same surface area as the particle, and the volume diameter is defined as the diameter of a sphere having the same volume as the particle. One of the most widely used derived
descriptors is the projected area diameter, which is the diameter
of a circle having the same area as the projected area of the particle resting in a stable position. The concept of projected area
diameter is illustrated in Figure 3c.
Several other derived descriptors of particle diameter have
been used for various applications. For instance, the sieve diameter is the width of the minimum square aperture through
which the particle will pass. Other descriptors that have been
used are the drag diameter, which is the diameter of a sphere having the same resistance to motion as the particle in a fluid of the
same viscosity and at the same velocity; the free-falling diameter,
which is the diameter of a sphere having the same density and
the same free-falling speed as the particle in a fluid of the same
density and viscosity; and the Stokes diameter, which is the freefalling diameter of a particle in the laminar-flow region.

Distribution of particle sizes

All analysts know that the particles that constitute real samples of powdered substances do not consist of any single type
but instead will generally exhibit a range of shapes and sizes.
Particle-size determinations therefore are undertaken to obtain information about the size characteristics of an ensemble
of particles. Furthermore, because the particles being studied
are not the exact same size, information is required about the
average particle size and the distribution of sizes about that
average.
One could imagine the situation in which a bell-shaped curve
is found to describe the distribution of particle sizes in a hypothetical sample; this type of system is known as the normal
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(a)

(b)
Cumulative distribution

Number frequency

20
15
10
5
0

100
80
60
40
20
0
0

Particle size (mm)

10 20 30 40

50 60

Particle size (mm)

Figure 4: Particle-size representations for a hypothetical normal distribution. Shown are (a) the
frequency distribution and (b) the cumulative distribution.

in each size fraction is identified, and

then one calculates the percentage of particles in each size fraction. This calculation yields the particle size histogram
(see Figure 4a). The number frequency
ordinarily is used to construct a cumulative distribution, which can be ascending or descending depending on the
nature of the study and what information is required (see Figure 4b).
The arithmetic mean of the ensemble
of particle diameters is calculated using
the relation
[3]

(b)

20

Number frequency

Number frequency

(a)

15
10
5
0

in which n is the number of particles

having a diameter equal to di. The standard deviation in the distribution then
is calculated using

20
15
10

[4]
5
0
10

In the example shown in Table I, one calculates that dav 5 30.2 mm and that s =
1.1.
The most commonly occurring value
Figure 5: Particle-size representations for a hypothetical log-normal distribution, plotted on a (a)
in the distribution is the mode, which is
linear scale and on a (b) logarithmic scale.
the value at which the frequency representation is a maximum value. The median divides the frequency curve into two equal parts and equals
Table I: Particle composition of a hypothetical sample
the particle size at which the cumulative representation equals
exhibiting a normal distribution.
50%. In a rigorous normal distribution, the mean, mode, and
median have the same value. For a slightly skewed distribution,
Size
Number
Number
Percent
Percent
however, the following approximate relationship holds:
(mm) in Band Frequency
Less Than Greater Than
0 10 20 30 40 50 60 70
Particle size (mm)

5
10
15
20
25
30
35
40
45
50
55
60
Total

50
90
110
280
580
600
540
360
170
120
60
40
3000

1.67
3.00
3.67
9.33
19.33
20.00
18.00
12.00
5.67
4.00
2.00
1.33
100

1.67
4.67
8.33
17.67
37.00
57.00
75.00
87.00
92.67
96.67
98.67
100.00

100

Particle size (mm)

98.33
95.33
91.67
82.33
63.00
43.00
25.00
13.00
7.33
3.33
1.33
0.00

distribution. Samples that conform to the characteristics of a

normal distribution are described fully by a mean particle size
and the standard deviation. Table I shows an example of a sample exhibiting a normal distribution in which 3000 particles
have been sorted according to an undefined determiner of their
size. In the usual data representation, the number of particles

[5]
It would be highly advantageous if powder distributions could
be described by the normal distribution function because all of
the statistical procedures developed for Gaussian distributions
could be used to describe the properties of the sample. However, unless the range of particle sizes is extremely narrow, most
powder samples cannot be described adequately by the normal
distribution function. The size distribution of the majority of
real powder samples usually is skewed toward the larger end of
the particle-size scale. Such powders are better described by the
log-normal distribution type. This terminology arose because
when the particle distribution is plotted by means of the logarithm of the particle size, the skewed curve is transformed into
one closely resembling a normal distribution (see Figure 5).
The distribution in a log-normal representation can be completely specified by two parameters: the geometric median particle size (dg) and the standard deviation in the geometric mean
Pharmaceutical Technology

DECEMBER 2001

43

in which n is the number of particles having particle size equal to di. Two samples
100
having identical dg and sg values can be
% mass
frequency
80
said to have been drawn from the same
20
% number
60
total population and exhibit properties
frequency
Cumulative
% mass
of characteristics of the total population.
40
10
Cumulative
In many applications, particle-size re20
% number
sults are processed by plotting the cu0
0
mulative frequency data on a logarith0
15 30 45 60
75
mic scale. If a straight line is obtained,
Size (mm)
Size (mm)
the particle-size distribution is said to
obey the log-normal function. The value
of dg is equal to the 50% value of the cuFigure 6: Particle-size representations for a hypothetical log-normal distribution. Shown are (a)
mulative distribution. The value of sg
the frequency distribution and (b) the cumulative distribution. Each contains the difference
is obtained by dividing the 84.1% value
obtained when processing the data in terms of either particle number or particle mass.
of the distribution by the 50% value.
Although the distribution in the lognormal representation is specified completely by the geometric median particle size and the geometric mean standard de(a) US
M
M
Ms
standard
s
viation, a number of other average values have been derived to
2,000
10
define useful properties. These values are especially useful when
12
1,500
16
the physical significance of the geometric median particle size
1,000
20
is not clear. The arithmetic mean (dav) particle size is defined
30
500
as the sum of all particle diameters divided by the total num40
400
ber of particles and is calculated using Equation 3. The surface
50
300
70
mean (ds) particle size is defined as the diameter of a hypo200
150
100
thetical particle having an average surface area and is calculated
140
100
using
200
(a)

(b)

Mesh (US standard sieve series)

% finer

% in bond

30

270
325
0.5 1 2

5 10

50
20 30 40 50 60 70 80 90 95 98 99 99.5

[7]

Cumulative percentage of undersize particles

(b) US

M
s

Mesh (US standard sieve series)

standard

The volume mean (dv) particle size is the diameter of a hypothetical particle having an average volume and is obtained from

Ms
2,000
1,500

10
12
16
20

1,000

30

[8]

500
400
300

40
50
70
100

200
150

140

100

The volume-surface mean (dvs) particle size is the average size

based on the specific surface per unit volume and is calculated
using

200
270
325
0.5 1 2

5 10

50
20 30 40 50 60 70 80 90 95 98 99 99.5

[9]

Cumulative percentage of undersize particles

Figure 7: Particle-size representations plotted in a log-probability

format for (a) a single hypothetical log-normal distribution and for
(b) a hypothetical sample containing two log-normal distributions
whose average particle size differs by ;50%.

(sg). The geometric median is the particle size pertaining to the

50% value in the cumulative distribution and is calculated using
[6]

44

Pharmaceutical Technology

DECEMBER 2001

For the distribution plotted in Figure 5, one can calculate that

dg 5 32.91 mm, dav 5 34.42 mm, ds 5 35.93 mm, dv 5 37.43 mm,
and dvs 5 40.62 mm.
Various types of physical significance have been attached to
the various expressions of particle size. For chemical reactions,
the surface mean is important, although for pigments the volume mean value is the appropriate parameter. Deposition of
particles in the respiratory tract is related to the weight mean
diameter, and the dissolution of particulate matter is related to
the volume-surface mean.
Particle-size distributions can be sorted according to the mass
(or volume) of the particles contained within a given size band
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Recommended reading
or to the number of particles contained in the same size R.R.Irani and C.F.Callis, Particle Size: Measurement, Interpretation, and Application (John
band. With substances having real density values, the disWiley & Sons,New York,1963).
Z.K.Jelinek,Particle Size Analysis (Ellis Horwood Ltd.,Chichester,1970).
tribution of the same ensemble of particles can look quite
different depending on how the data are plotted. Figure J.D.Stockham and E.G.Fochtman, Particle Size Analysis (Ann Arbor Science Publishers,
6 shows the frequency and cumulative distribution plots
Ann Arbor,MI,1977).
for the same sample, but the data have been separately B.H.Kaye,Direct Characterization of Fine Particles (John Wiley & Sons,New York,1981).
H.G.Barth,Modern Methods of Particle Size Analysis (John Wiley & Sons,New York,1984).
processed in terms of the mass and particle numbers.
T.Allen,Particle Size Measurement, 5th ed.(Chapman and Hall,London,1997).
Unfortunately not every powdered sample is characterized by the existence of a single distribution, and the
character of real samples can be quite complicated. Recogniz- recommended references to additional information (see Recing the existence of multimodal distributions is not always a ommended reading sidebar). Most highly recommended are
straightforward process, but their existence often can be detected the various editions of Particle Size Measurement by Allen beby plotting the data on log-probability paper. The existence of cause they contain some of the most detailed and informative
more than one particle population is indicated by a change in expositions available about these topics. However, the scope of
the slope of the line. Figure 7 shows a single log-normal distri- the discussion in this opening article provides a sufficient basis
bution and a multimodal sample consisting of two populations for the expositions of the various methodologies that will folwhose mean differed by approximately 50%. The break in the low in subsequent installments of this column.
log plot is clearly evident, but if one were to simply plot the latter sample in either a frequency or cumulative view, one would References
1. H.G. Brittain, What is the Correct Method to Use for Particle-Size
not have been able to detect the existence of two particle-size
Determination? Pharm. Technol. 25 (7), 9698 (2001).
populations in the sample.

Summary
This rather simplified discussion of particle shape, size, and distribution represents only an introduction to the topic. Interested readers should consult the primary sources in the list of

2. Optical Microscopy, General Test ^776&, USP 24 (The United States

Pharmacopoeial Convention, Rockville, MD, 2000), pp. 19651967.
3. T. Allen, Particle Size Measurement (Chapman and Hall, London, 3rd
ed.,1981) pp. 107120.
4. H. Heywood, J. Pharm. Pharmacol. (S15) 56T, (1963). PT

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