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Particle size analysis

Measurement techniques

WHY IS PARTICLE SIZE ANALYSIS IMPORTANT?

.

2.1 PARTICLE SIZE AND SHAPE

• Particle size: refers to one particle.

• Precise particle size is difficult to obtain due to

the irregular shape of particles.

• For spherical particles, defining particle size is

easy; it is simply the diameter of the particle.

• For non-spherical particles, the term

"diameter" is strictly inapplicable. For example,

what is the diameter of a flake or a fiber?

• Also, particles of identical shape can have

quite different chemical composition and,

therefore, have different densities.

• The differences in shape and density could

introduce considerable confusion in defining

particle size.

• Equivalent diameter is often used.

sphere with the same volume (mass) as the

particle:

d v = 6V / π 3

sphere with the same surface area as the

particle (BET isotherm):

Chee 3920: Particle Size and Shape 4

ds = A / π

A … real particle surface area.

diameter - diameter of a sphere with the

same volume to surface area ratio as the

particle.

d Sauter = 6V / A

V and A … real particle volume and surface

area.

Chee 3920: Particle Size and Shape 5

Example of equivalent diameters for a particle

with a shape of rectangular box

Dimension (mm) 20 x 30 x 40

2

Surface area (mm ) 5200

3

Volume (mm ) 24000

dv (mm) 35.8

ds (mm) 40.7

dSauter (mm) 27.7

- Stokes (hydraulic) diameter – from settling

velocity (drag force and weight) – diameter

of a sphere with the same density and

terminal settling velocity (discussed later).

18µU

d Stokes =

g (ρ −δ )

µ … liquid viscosity

µ = 0.001 Pa/s for water

µ = 0.00001 Pa/s for air

2

g … acceleration due to gravity (9.81 m/s )

3

ρ = 2500 kg/m for quartz (SiO2)

3

δ = 1000 kg/m for water.

sieve aperture through which particles pass.

Chee 3920: Particle Size and Shape 8

• Microscopically Observed Shapes

particle image –always taken in the same

direction.

tangents –always taken in the same direction.

same area of the particle image.

with the same perimeter of the particle image.

• Deviation of irregular shape from spheres.

Is described by sphericity.

ψ V = π ( dV ) / A

2

A is the real surface area.

ψ A = π ( d A ) / ( 6V )

3

where d A is surface-equivalent diameter

V is the real volume.

ψ VA = π ( d32 ) / A

2

ψ AV = π ( d32 ) / ( 6V )

3

• Equivalent diameter of many particles

- Mean diameter, d

m

d = ∑ γ i di

i =1

γ i is mass fraction of i-th size range.

- Volume equivalent diameter, dV

m

( dV ) = ∑ γ i di

3 3

i =1

- Surface equivalent diameter, d A

m

(dA ) = ∑ γ i di

2 2

i =1

∑γ d

3

i i

d32 = i =1

m

∑γ d

2

i i

i =1

2.2 METHODS OF PARTICLE SIZE ANALYSIS

Table 2.1 Some methods of particle size analysis

Method Equivalent size

Test sieving 100 mm – 10 microns

Elutriation 40 microns – 5 microns

Gravity sedimentation 40 microns – 1 microns

Centrifu. sedimentation 40 microns – 50 nano

Microscopy 50 microns – 10 nano

Ligth scattering 10 microns – 10 nano

Sieve Analysis

Chee 3920: Particle Size and Shape 14

- Good for particle >25 µm, cheap & easy.

- Carried out by passing sample via a series of

sieves (Fig 2.1)

- Weighing the amount collected on each sieve

- With wet or dry samples.

• Test sieves

• Designed by the norminal aperture size (Fig

2.2)

• Popular designs: BSS (British), Tyler series

(American), DIN (German).

Largest

apertur

Smallest

aperture

Chee 3920: Particle Size and Shape 16

Mesh = number of apertures per inch

Chee 3920: Particle Size and Shape 17

Fig 2.2 Examples of aperture designs (Wills)

Presentation of results for sieve analysis

Size range Mid-point Mass Mass fraction Cumulative Cumulative

retained undersized Oversized

(micron) (micron) (g)

+200 200 0 0 1.000 0.000

200 - 150 175 10 0.111 1.000 0.000

150 - 100 125 40 0.444 0.889 0.111

100 - 50 75 30 0.333 0.444 0.556

50 - 0 25 10 0.111 0.111 0.889

0 0 0 0.000 1.000

sum 90

Gravity sedimentation technique

• Uses the dependence of the settling velocity

on the particle size (the Stokes law)

du

mg − m ' g − F = m

dt

st nd

where the 1 term is the particle weight, the 2

rd

is the buoyancy, 3 is the drag force and the

last term is the inertial force. u is particle

velocity.

Chee 3920: Particle Size and Shape 20

• (Terminal) settling velocity:

u=

( ρ − δ ) gd 2

18µ

where ρ and δ are particle and liquid density, g

is gravity acceleration and µ is liquid viscosity.

• Experimental steps:

- Sample is uniformly dispersed in water in a

beaker.

- A siphon tube is immersed into 90% of the

water depth.

Chee 3920: Particle Size and Shape 21

- Particle with size d is sucked from the beaker

at time interval t calculated from the

immersed depth and Stokes’ velocity: t = h / u .

decantation

for gravity

sedimentation

size analysis

(Wills)

Chee 3920: Particle Size and Shape 22

Pipette filler to

collect the sample

Two-way stopcock

pipette for

sedimentation size

analysis (Wills)

Chee 3920: Particle Size and Shape

Elutriation technique

• Uses an upward current of water or air for

sizing the sample.

• Is the reverse of gravity sedimentation and

Stokes’s law applies.

• Particles with lower settling velocity overflow

• Particles with greater velocity sink to under

flow.

• Sizing is achieved with a series of simple

elutriators (Fig 2.5).

Chee 3920: Particle Size and Shape

Fig 2.5 Simple

elutriator

(Wills)

Chee 3920: Particle Size and Shape

• For fine particles (<10 microns), cyclosizer is

usually used (Fig 2.6).

Chee 3920: Particle Size and Shape

Microscopy techniques

• Used for small (dry) samples.

• Particle size is directly measured.

• Optical microscopes: 1 micron (wavelength of

light is ~ 100 microns)

• Electron (TEM and SEM): ~ 10 nm.

Light scattering techniques

• Based on the capability of colloidal particles to

scatter light.

• Useful for colloidal particles.

• Static light scattering: Intensity ~ particle

volume and particle concentration.

• Dynamic light scattering measurements give

2

the r.m.s. of displacements, x .

• Brownian diffusivity, D, of particles is

determined from the Einstein-Smoluchowski

Chee 3920: Particle Size and Shape 21

equation

x 2

= 2 Dt

equation

3πµ d = k BT / D

where µ is liquid viscosity

kB is Boltzman’s constant

T is absolute temperature.

2.3 ANALYSIS OF SIZE DISTRIBUTION

(Of many particles)

• Based on tabular results of size analysis

(Table 2.2)

• Characteristic parameters: mean diameter,

standard deviation, distribution functions, and

cumulative curves.

• Mean diameter (shown previously)

m

d = ∑ γ i di

i =1

• Standard deviation, σ,

m m

σ = ∑ γ i ( di − d ) = ∑ γ i di − ( d ) = ( di ) − ( d )

2 2 2 2 2 2

i =1 i =1

• Frequency distribution

- Histogram: mass of size range versus size

range.

- Normalised histogram: mass fraction vs size

range.

- Continuous distribution function: mid-points of

mass fraction vs mid-points of size range

Chee 3920: Particle Size and Shape 24

40

Mass versus size range

30

20

10

0

0 - 50 50 - 100 100 - 150 150 - 200

Size range (micron)

0.5

Mass fraction versus size range

0.4

0.2

0.1

0

0 - 50 50 - 100 100 - 150 150 - 200

Size range (micron)

0.5

0.4

Midpoint of mass fraction versus

midpoint of size range

0.3

f(d)

0.2

0.1

0

0 50 100 150 200

d (microns)

(Data in Table 2.3)

Chee 3920: Particle Size and Shape 27

- Theoretical distribution functions (taken from

theory on probability and statistics)

1

1 d − d

2

f (d ) = exp −

σ 2π 2 σ

σ … standard deviation of the distribution

d … mean (median) diameter

∞

Property: ∫ f ( d ) dd = 1

−∞

or ∑ f ( d ) ∆d = 1 .

i

2.5

1 d −d

2

1

f (d ) = exp −

σ 2π

2 σ

2

Experiments

1.5

f(d)

0.5

0

0 50 100 150 200

d (microns)

frequency distributions. d = 100 µ m & σ = 20

Chee 3920: Particle Size and Shape 29

Log-normal distribution

1

1 x − x

2

f ( x) = exp −

σ 2π 2 σ

where x = log ( d ).

σ … standard deviation of the distribution

d … mean (median) diameter

∞

Property: ∫ f ( x ) dx = 1

−∞

or ∑ f ( x ) ∆x = 1 .

i

2.5 2.5

( )

log ( d ) − log d

2

1 1

f (d ) = exp −

σ 2π 2

σ

2 2

1.5 1.5

f(d)

f(d)

1 1

0.5 0.5

0 0

0 50 100 150 200 0.5 1.5 2.5

d (microns)

log(d/microns)

distributions in the normal (left) and log-normal

(right) diagrams. log ( d / µm) = 1.6 & σ = 0.17 .

Chee 3920: Particle Size and Shape 31

Comments:

Many size distributions do not follow the

theoretical Gaussian and log-normal statistics.

describing the particle size distributions. We

need the mean (median) diameter and the

standard deviation.

for the particle size distributions (shown later).

Chee 3920: Particle Size and Shape 32

• Viewing distributions

No details of fines

can be seen in the

normal-normal plot

gives more details

of fines

• “Average” size of many particles

Mode – most frequent size occurring

Median – d50 (50% cumulative distribution)

Means – different types for different uses

- Arithmetic mean

- Quadratic mean

- Geometric mean

- Harmonic mean

Graphical correlations (M Rhode, 1998)

Chee 3920: Particle Size and Shape 35

n

d + d 2 + ... + d n ∑d i

Arithmetic mean d= 1

n

= i =1

( d1 ) + ( d 2 ) + ... + ( d n )

2 2 2

1 n

Quadratic mean ( d ) ∴ ∑ i ( )

2

d=

2

= d

n n i =1

1/ n

1 1 1

+ + ... + n

1 d1 d 2 dn d=

Harmonic mean d

=

n ∴ n

∑ (1/ d ) i

i=1

Modes of distributions

f(d)

- Mono disperse particles

0.5

0.4

0.3

f(d)

0.2

0.1

0

0 50 100 150 200

d (microns)

- Bimodal distributions (Fig 2.8 – solid line)

3

f(d) 2

0

0 50 100 150 200

d (microns)

mixtures of two minerals.

Chee 3920: Particle Size and Shape 38

For analysis, bimodal distribution is separated

(using an appropriate mathematical technique

called deconvolution) into the Gaussian/log-

normal distributions.

• Cumulative distributions

- Undersized cumulative distribution

m

Q ( di ) = ∑ γ i

i =1

Chee 3920: Particle Size and Shape 39

- Oversized cumulative distribution

1

P ( di ) = ∑ γ i = 1 − Q ( di ).

i =m

Size range Mid-point Mass Mass fraction Cumulative Cumulative

retained undersized Oversized

(micron) (micron) (g)

+200 200 0 0 1.000 0.000

200 - 150 175 10 0.111 1.000 0.000

150 - 100 125 40 0.444 0.889 0.111

100 - 50 75 30 0.333 0.444 0.556

50 - 0 25 10 0.111 0.111 0.889

0 0 0 0.000 1.000

sum 90

1.000

Oversized

Undersized

0.800

0.400

0.200

0.000

0 50 100 150 200

d (microns)

Chee 3920: Particle Size and Shape 41

- Many curves of cumulative oversized and

undersized distributions versus particle size

are S-shaped.

- Two approximations for cumulative

distributions are known, i.e., Rosin-Rammler

and Gates-Gaudin-Schuhmann distributions.

d n

P ( d ) = exp −

d '

Chee 3920: Particle Size and Shape 42

where d ' and n are parameters.

d ' and n can be determined from the graph

of log {− ln ( P )} versus log ( d ) in the log-log

diagram which gives a straight line

{ }

log − ln P ( d ) = n log ( d ) − n log ( d ')

-nlog(d’) … intercept of the straight line.

1 1

0.8 0

log{-ln[P(d)]}

0.6 -1

P(d)

0.4 -2

0.2 -3

0 -4

0 50 100 150 200 0 1 2 3

d (microns) log(d/micron)

The slope of the log-log diagram gives n = 2.

The intercept is equal to –4 and gives d’ = 100 microns.

- Gates-Gaudin-Schuhmann (GGS) distribution

Q ( d ) = const × ( d / d ')

n

n < 1 represents samples with decreasing coarse fractions.

Q(d)

n<1

n =1

n>1

d

Chee 3920: Particle Size and Shape 45

• Relationship between frequency and

cumulative distributions

d d min

P(d ) = ∫ f ( x ) dx ; Q ( d ) = ∫ f ( x ) dx .

d max d

Differential relationships:

dP

= f ( d ) => f(d) is also called differential frequency distribution!

dd

dQ

= − f (d )

dd

• Comparison of number, volume & surface

distributions

Many instruments measure number distribution but we want

surface area or volume distribution

(M Rhode, 1998)

Conversions

Surface distribution: f s ( d ) = k S d f N ( d )

2

3

∞

∫ f ( d ) dd = 1

0

density with size.

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