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Fundamentals
Lesson 2
Methods of Particle Size
Measurements
Sieving
• Dry sieving using woven wire sieves is a simple, cheap
method of size analysis (>45µm). Sieving gives a mass
distribution and a size known as the sieve diameter.
• Since the length of the particle does not hinder its passage
through the sieve apertures (unless the particle is extremely
elongated), the sieve diameter is dependent on the maximum
width and maximum thickness of the particle.
• The most common modern sieves are in sizes such that the
ratio of adjacent sieve sizes is the fourth root of two
( 4 𝑎)fourth root of two (eg. 45, 53, 63, 75, 90, 107µm).
• Sieving gives reliable and reproducible size analysis.
• Air jet sieving, in which the powder on the sieve is fluidized
by a jet or air, can achieve analysis down to 20µm. Analysis
down to 5µm can be achieved by wet sieving, in which the
powder sample is suspended in a liquid.
Sieving
• Weight distribution
• Sieve analysis is performed using a nest
or stack of sieves where each lower
sieve has a smaller aperture size than
that of the sieve above it.
• Sieves can be referred to either by their
aperture size = mesh size = sieve
number (BP, PhEur)
• US: The mesh size is the number of
wires per linear inch.
– 250 m = No. 60
– 125 m = No. 120
• Approx. size range : 5µm - ~3mm
– Standard woven wire sieves
– Electroformed micromesh sieves at
the lower end or range (< 20µm)
– Punch plate sieves at the upper range 8
• Sieving may be performed wet or dry, by machine or by hand, for a fixed time
or until powder passes through the sieve at a constant low rate
• Machines:
– Shaking
– Vibration
– Use a jet of air to clear the sieves
– Ultrasonics (wet sieving)
• Wet sieving
• Air-jet sieving
• Advantages
– Easy to perform
– Wide size range
– Inexpensive
• Disadvantages
– Irreproducibility
– Wear/damage in use or cleaning
– Irregular/agglomerated particles
– Rod-like particles : overestimate of
under-size
– Labour intensive
6
British Pharmacopoeia Volume V Appendix XVII A.
Particle Size of Powders Particle size classification of
powders
(Ph. Eur. method 2.9.12, Sieve test)
o Coarse powder: Not less than 95% by mass passes through a number
1400 sieve and not more than 40 % by mass passes through a number
355 sieve.
o Moderately fine powder: Not less than 95% by mass passes through a
number 355 sieve and not more than 40% by mass passes through a
number 180 sieve.
o Fine powder: Not less than 95% by mass passes through a number 180 sieve
and not more than 40% by mass passes through a number 125 sieve.
United States Pharmacopeia
General Chapters: <811> POWDER FINENESS
8
Microscopy
• The optical microscope may be used to measure particle sizes
down to 5 μm. For particles smaller than this diffraction causes
the edges of the particle to be blurred and this gives rise to an
apparent size.
• Disadvantages • Disadvantages
– Time consuming - high operator – Very expensive
fatigue - few particles examined* – Time consuming
– Very low throughput sample preparation
– No information on 3D shape – Materials such as emulsions
– Certain amount of subjectivity difficult/impossible to
associated with sizing - operator prepare
bias – Low throughput - Not for
* Overcome with (semi-)automated image routine use
analysis systems
Sedimentation
• In this method, the rate of sedimentation of a sample
of particles in a liquid is considered.
• The suspension is dilute and so the particles are
assumed to fall at their single particle terminal
velocity in the liquid (usually water). Single particle
Reynold’s number
• Stokes’ law is assumed to apply (Rep < 0.3) and so
the method using water is suitable only for particles
typically less than 50 μm in diameter.
• The rate of sedimentation of the particles is
followed by plotting the suspension density at a
certain vertical position against time. In chemistry, a suspension is a
heterogeneous mixture
• The suspension density is directly related to the containing solid particles that
cumulative undersize and the time is related to the are sufficiently large for
particle diameter via the terminal velocity. This is sedimentation. Usually they
demonstrated in the following: must be larger than one
micrometer.
• Referring to Figure, the suspension density is sampled at a
vertical distance, h below the surface of the suspension. The
following assumptions are made:
x – Stokes diameter
µ - Viscosity (pure liquid medium)
ρp – Density of the solid particles
ρf – Density of the pure liquid
g – Gravitational acceleration
h – Distance from liquid level to the suspension sampling level
t – time taken for particle travel along h distance
• Particles smaller than x will travel slower than h/t and will still be in
suspension at the sampling point.
• The particle size measured is the Stokes’ diameter, i.e. the diameter
of a sphere having the same terminal settling velocity in the Stokes
region as the actual particle.
• Stokes Law states that the speed or velocity with which particles
settle out of a liquid medium is dependent on the radius of the
particles. The bigger the particle, the faster it will fall out of
suspension.
• A common form of this method is the Andreason pipette which is capable of
measuring in the range 2–100 μm. At size below 2 μm, Brownian motion
causes significant errors.
• The labour involved in this method may be reduced by using either light
absorption or X-ray absorption to measure the suspension density.
Where −∆𝑝 is the pressure drop across the bed, ε is the packed bed
void fraction, H is the depth of the bed, µ is the fluid viscosity and U is
the superficial fluid velocity.
Problem :
(1) Determine the surface –volume mean diameter and
(2) the specific surface of the powder sample.
Exercise 3
Water flows through 3.6 kg of glass particles of density 2590 kg/m3 forming a
packed bed of depth 0.475 m and diameter 0.0757 m. The variation in
frictional pressure drop across the bed with water flow rate in the range 200-
1200 cm3/min is shown in columns one and two in Table below.
Given formula:
−∆𝑝 1−𝜀 2 𝜇𝑈
= 180
𝐻 𝜀3 𝑥𝑠𝑣 2
𝑥𝑈𝜌𝑓
Reynolds number, 𝑅𝑒 ∗ =
𝜇 1−𝜀
Prepared by:
Dr. Ng Ching Yin
ngcy@ucsiuniversity.edu.my