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Part I

Particle Characterization and


Measurement

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1.1 Particle Size
JunIchiro Tsubaki
Nagoya University, Nagoya, Japan

1.1.1 DEFINITION OF PARTICLE DIAMETER


Particle size data are essential to anyone treating powders. Expressing the size of a single particle
is not a simple task when the particle is nonspherical. Expressions of individual particle size and a
hypothetical equivalent sphere with regard to some properties. Table 1.1 lists the physical meaning
of variously defined characteristic diameters.
When a particle is circumscribed by a rectangular prism with length l, width w, and height t, its
size is expressed by the diameter, obtained from the three dimensions. l, w, and t are measured with
a microscope. Feret and Martin diameter are statistical diameters, which are affected by the particle
orientation or measuring direction. The mean values of them are often defined as characteristic
diameters. Unrolled diameter is the mean value of a statistical diameter.
The equivalent diameters are the diameters of spheres having the same geometric or physical
properties as those of nonspherical particles.

1.1.2 PARTICLE SIZE DISTRIBUTION


Size Distribution
When a certain characteristic diameter, shown in Table 1.1, is measured for N particles, and the
number of particles, dN, having diameters between x and x + dx, is counted, the density size distri-
bution q 0 (x) is defined as

dN 1
qo ( x )  (1.1)
N dx

where


∫ q ( x ) dx  1 (1.2)
0 0

The cumulative distribution Q0(x) is given as

Q0 ( x )  ∫ q0 ( x ) dx
x
(1.3)
0

Therefore,

dQ0 ( x )
 q0 ( x ) (1.4)
dx

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4 Powder Technology Handbook

TABLE 1.1 Expression of Particle Size


Definition of characteristic diameters Physical meaning and corresponding
measuring method
Geometric Breadth: b
size Length: l
Thickness: t
1/ 3 1/ 2
b 1 b  l  t ⎛ b ⎞ 3 ⎛ 2lb  2bt  2lt ⎞
, ,⎜ ⎟ , , lb ⎜ ⎟⎠
2 3 ⎝t⎠ 1 / l 1 / b ⎝ 6

Feret diameter Distance between pairs of parallel tangents


to the particle silhouette in some fixed
direction

Martin diameter Length of a chord dividing the particle


silhouette into two equal areas in some
fixed direction

Unrolled diameter Chord length through the centroid of the


particle silhouette

Sieve diameter a1, a2: Openings of sieves

(a  a2 ) or a1a2
1
2 1

Volume: v Equivalent Equivalent projection area Diameter of the circle having same area as
diameter diameter (Heywood diameter) projection area of particle, corresponding to
diameter obtained by light extinction
Surface: s Equivalent surface area diameter Diameter of the sphere having the same
(specific surface diameter) surface as that of a particle
(s/p)1/2
Equivalent volume diameter Diameter of the sphere having the same
(6v/p)1/3 volume as that of a particle, corresponding
to diameter obtained by (electrical sensing
zone method)
Stokes diameter Diameter of the sphere having the same
gravitational settling velocity as that
of particle obtained by gravitational or
centrifugal sedimentation and impactor
Aerodynamic diameter Diameter of the sphere having unity in
specific gravity and the same gravitational
settling velocity as that of a particle
obtained by the same methods as above
Equivalent light-scattering Diameter of the sphere giving the same
diameter intensity of light scattering as that of a
particle, obtained by the light-scattering
method

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Particle Size 5

The size distributions thus defined are on a number basis. In the case of mass or volume basis,
total mass M and fractional mass dM are used instead of N and dN, respectively, and also the sub-
script value is changed from 0 to 3, so that q3(x), Q3(x) should be used. In general the subscript is
described as r, and r  0, 1, 2, 3 corresponds to number, length, area, and mass or volume basis,
respectively. Density distribution qr (x) can be transformed to another basis distribution qr(x) by

x sr qr ( x ) dx
qs ( x )  (1.5)
x sr qr ( x ) dx

∫0

When particle size distributes widely, the distributions are plotted versus ln x instead of x and
defined as

Qr ( ln x )  Qr ( x ) (1.6)

dQr ( x )
q∗r (ln x )   xqr ( x ) (1.7)
d ln x

The density distribution in a representation with a logarithmic abscissa is distinguished by


superscript *.
The discrete expression, which gives the size distribution histogram, q–r,i, q–*r,i, becomes

Q r , i Qr ( xi )  Qr ( xi1 )
q r,i   (1.8)
xi xi  xi1

∗ Qr ,i Qr ( xi )  Qr ( xi1 )
q r ,i   (1.9)
 ln xi ln( xi xi1 )

Normal Distribution
The normal or Gaussian distribution function is defined as

1 ⎡ ( x  x )2 ⎤
qr ( x )  exp ⎢ ⎥
50
(1.10)
⎢⎣ ⎥⎦
2
s 2p 2 s

where x 50 is the 50% or median diameter defined as Qr (x50 )  0.5 and  is the standard deviation
expressing the dispersion of the distribution.

s  x84.13  x50  x50  x15.87 (1.11)

Log-Normal Distribution
The log-normal distribution function is given by substituting ln x and ln g, respectively, for x and
 in Equation 1.10 as follows:

1 ⎡ ( ln x  ln x )2 ⎤

q r (ln x )  exp ⎢ 50
⎥ (1.12)
ln s g ⋅ 2p ⎢⎣ 2 ln 2 s g ⎥⎦

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6 Powder Technology Handbook

where g is the geometric standard deviation given as

x84.13 x
sg   50 (1.13)
x50 x15.87

If a size distribution obeys the log-normal form, the other distribution converted by Equation 1.5
also obeys the log-normal form. The geometric standard deviation of any distribution is the same
value; meanwhile, the median diameters are different but can convert each other. In the case of the
volume and number distribution the median diameters, x50,3 , x50,0, , can convert each other by Hatch’s
equation.

ln x50,3  ln x50,0  3 ln 2 s g (1.14)

Rosin–Rammler (Weibull) Distribution


The Rosin–Rammler or Weibull distribution function is written as

⎡ ⎛ x ⎞n⎤
Qr ( x )  1  exp bx( n
) or Qr ( x )  1  exp ⎢ ⎜ ⎟ ⎥
⎢⎣ ⎝ xe ⎠ ⎥⎦
(1.15)

where b is a constant equal to xe–n and x e is an absolute size constant defined as x e  x 63.2 , that is,
xe  x63.2 . n is the distribution constant expressing the dispersion of particle sizes. The density
distribution is written as

1⎛ x ⎞
n
⎡ ⎛ x ⎞n⎤
qr ( x )  nbx n1
exp(bx ) or qr ( x )  ⎜ ⎟ exp ⎢ ⎜ ⎟ ⎥
n
(1.16)
x ⎝ xe ⎠ ⎢⎣ ⎝ xe ⎠ ⎥⎦

Graphical Representation
As an example, a set of data obtained by a sieving test is illustrated in Table 1.2, and the size dis-
tributions are illustrated in Figure 1.1 with a general abscissa and Figure 1.2 with a logarithmic
abscissa.
Q3,i in Table 1.2 is plotted on log-normal and Rosin–Rammler probability paper, as shown in
Figure 1.3. Since the plots are on a straight line on a log-normal probability graph, the particle size
distribution obeys the log-normal function of which x50  1.0 mm and x84.13  2.2 mm. If we read the
two values of x15.87, x50 or x84.13, g can be calculated. From Figure 1.3 x50  1.0 mm and x84.13  2.2 mm,
then g  2.2. The dotted line in Figure 1.3 is the number distribution converted from measured volume
distribution by Hatch’s equation.
ISO 9276-1 (JIS Z 8819-1) standardizes the graphical representation of particle size analysis data.

1.1.3 AVERAGE PARTICLE SIZE


All average particle diameters except the geometric mean diameter are defined by

M kr ,0 M kr3,3
x k ,r  k M k ,r  k k (1.17)
Mr ,0 Mr3,3

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Particle Size 7

TABLE 1.2 Calculation of the Histogram and the Cumulative Distribution


1 2 3 4 5 6 7 8
i xi Mi Q3,i xi q–3,i lnxi (q–3,i)
(mm) ( 10–3kg) (%) (mm) (%mm–1) (%)
0 0.063 0
1 0.09 0.1 0.1 0.027 3.7 0.357 0.3
2 0.125 0.27 0.37 0.035 7.7 0.329 0.8
3 0.18 1.03 1.4 0.055 18.7 0.365 2.8
4 0.25 2.2 3.6 0.07 31.4 0.329 6.7
5 0.355 5.4 9 0.105 51.4 0.351 15.4
6 0.5 9.3 18.3 0.145 64.1 0.342 27.2
7 0.71 13.7 32 0.21 65.2 0.351 39.1
8 1 17 49 0.29 58.6 0.342 49.6
9 1.4 17 66 0.4 42.5 0.336 50.5
10 2 14.6 80.6 0.6 24.3 0.357 40.9
11 2.8 9.9 90.5 0.8 12.4 0.336 29.4
12 4 5.6 96.1 1.2 4.7 0.357 15.7
13 5.6 2.4 98.5 1.6 1.5 0.336 7.1
14 8 1.1 99.6 2.4 0.5 0.357 3.1
15 11.2 0.3 99.9 3.2 0.1 0.336 0.9
16 16 0.1 100 4.8 0.0 0.357 0.3

Where Mk,r is complete kth moment of a qr (x) -distribution.


M k ,r  ∫ x k qr ( x ) dx (1.18)
0

Geometric mean diameter is defined as


ln x geo, r  ∫ ln x ⋅ qr ( x ) dx (1.19)
0

Although a lot of average diameters can be defined, the several listed in Table 1.3 are generally used.
If a density distribution is given as a histogram, Mk,r is calculated by the following equations.
Equation 1.18 is rewritten as follows if k  –1.

xi

∫ x dx  k 1 ∑ q ( x )
m m
1
M k ,r  ∑ q r ,i k
r ,i
k1
i  xik11
i1 xi1 i1

⎛ xik1  xik11 ⎞ (1.20)


1 m
 ∑ r ,i ⎜⎝ x  x ⎟⎠
k 1 i1
ΔQ
i i1

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8 Powder Technology Handbook

100

80 Q3
q* [%], q* [%], Q [%]
3

60

q
3

40
3

q
20 3

0
0.1 1 10
x [mm]

FIGURE 1.1 A graphical representation of particle size distribution with a linear abscissa.

If k  –1,

x
m m
ln i
xi xi1
M1,r  ∑ q r ,i ln  ∑ Qr ,i (1.21)
i1 xi1 i1 xi  xi1
.

Equation 1.19 is rewritten as follows:

m xi m
q r ,i m
Qr ,i
ln x geo, r  ∑ q r ,i ∫ ln xdx  ∑ x  x ∑ (1.22)
i1 xi1 i1 i i1 i1 ( xi  xi1 )2

The values of the average diameters listed in Table 1.3 can be calculated from the data in Table 1.2.
The calculation results are illustrated in Table 1.3.
The spread of a size distribution is represented by its variance, which represents the square of the
standard deviation, . The variance, 2 , of a qr (x) -distribution is defined as

( x  x ) q ( x)dx  M ( )
 2
2  ∫
2

1,r r 2 ,r  M1,r (1.23)


0

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Particle Size 9

100
Q3

80
q* [%mm–1], q* [%mm–1], Q3 [%]

q3

60
3

40
3

20

q3
0
0 2 4 6 8 10
x [mm]

FIGURE 1.2 A graphical representation of particle size distribution with a logarithmic


abscissa.

From a histogram,

2
1⎡ m ⎤ 1⎡ m ⎤
( ) ( )
  ⎢ ∑ q r ,i x 3i  x 3i1 ⎥  ⎢ ∑ q r ,i x i2  x i21 ⎥
2

3 ⎣ i1 ⎦ 4 ⎣ i1 ⎦ (1.24)


1⎡ m ⎛ x  x i1 ⎞ ⎤ 1 ⎡ m
3 3 2

 ⎢ ∑ Qr ,i ⎜ i ⎟ ⎥ − ⎢ ∑ r ,i ( i
 Q x  xi1 )⎥
3 ⎢ i1
⎣ ⎝ xi  xi1 ⎠ ⎥⎦ 4 ⎣ i1 ⎦

The standard deviation of the particle sizes illustrated in Table 1.2 is calculated as  1.29 mm by
Equation 1.24.
ISO 9276–2 (JIS Z 8819-2) standardizes the calculation of average particle sizes.

Notation
i number of the size class with upper particle size xi
k power of x
m total number of size classes
Mk,r complete kth moment of a qr (x) -distribution
n distribution constant

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99.9 99.9
99 99
90 90
70 70
50 50
30 30
20
Q0.Q3 [%]

20

Q3 [%]
10 10
5 5

1 1

0.1 0.1
0.01 0.1 1 10
x [mm]

FIGURE 1.3 Cumulative distributions on a log-normal and Rosin–Rammler distribution


graph.

TABLE 1.3 Average Diameters


Average diameters Symbols Definition Examples of
q0(x) q3(x) Table 1.2 [mm]
from from
Arithmetic average length diameter x–1,0 0.228
Weighted average number diameter
Arithmetic average surface diameter x–2,0 0.303
Arithmetic average volume diameter x–3,0
0.410
Weighted average length diameter x–1,1 0.402
Weighted average surface diameter, x–1,2
0.749
Sauter-diameter
Weighted average volume diameter x–1,3 1.40
Harmonic mean diameter x–
1,r
0.147 (r0)
0.749 (r3)
Geometric mean diameter x–geo,r 3.98 (r3)

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Particle Size 11

N particle number
qr(x) density distribution
qr  qr(x)
qr*(ln x) density distribution in a representation with a logarithmic abscissa
q r* qr*(x)
q–r,i average density distribution of the class Δ xi , histogram
q–r,i average density distribution of the class Δ In xi, histogram
Qr(x) cumulative distribution
Qr  Qr(x)
ΔQr,i  Qr(xi)Qr(xi1)
x particle size, diameter of a sphere
xe absolute size constant
xi upper size of a particle size interval
xi1 lower size of a particle size interval
Δ xi xixi1, width of the particle size interval
x15.87, x50, x63.2, x84.13 defined as Qr(x15.87)  0.1587,Qr(x50)  0.5 ,Qr(x63.2)  0.632 Qr(x84.13)  0.8413
x50,3 median particle size of a cumulative volume distribution
x50,0 median particle size of a cumulative number distribution
r, s type of quantity of a distribution, r, s  0, 1, 2, 3
s standard deviation
sg geometrical standard deviation of log-normal distribution

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