PARTICLE SIZE ANALYSIS

& BET ADSORPTION

Presented by
Joshwa Joji
 PARTICLE SIZE ANALYSIS
• The PSD of a material affects the strength and load-bearing properties, reactivity of solids
participating in chemical reactions etc in the manufacture of printer toner, cosmetics, and
pharmaceutical products.

• Particle size has a profound impact on different processes such mixing, drying, blending, coating
etc.

• Large number of methods for the determination of particle size available, not expected to give
identical results. The size of a particle depends on the method used for its measurement.
Some of the particle size determination methods;

1. Optical microscopy
2. Sieving method
3. Sedimentation method
4. Optical and electrical sensing zone method
5. Laser light scattering techniques
6. Surface area measurement techniques (BET)
 Optical Microscopy

• Ordinary optical microscope are used for particle

size of 0.2 µm to about 100 µm.

• The microscope eyepiece/mechanical stage is

fitted with a micrometre

• Photograph of slide is taken or project particles

on the slide onto a screen
Sieving Method

• Uses a series of sieves calibrated by the

National Bureau of Standards

• This ‘nest’ of sieves is vibrated until the

residue on each sieve can pass through the
upper sieve but cannot pass through the
lower sieve.
 Sedimentation Method
• Measurement of rate of settling of particles which are uniformly dispersed in a fluid.

• Particle size is expressed via stokes diameter which is referred to as the diameter of an
equivalent sphere having the same rate of sedimentation of the irregular particles.

• Sedimentation of the particles can be studied using Andreasian pipette

• The particles must not be aggregated or clumped together in the suspension,
for this a deflocculating agent is added.

• The rate of sedimentation of the particles must not be rapid that turbulence
is set up because this in turn will affect sedimentation

• Stokes law cannot be used if Reynolds no is greater than 0.2

• The equation holds true for only spheres falling freely without any hindrance
and at a constant rate
 Why surface area?
Surface area directly correlates with desired properties.

• Reactivity
• Dissolution
• Catalysis
• Separation

 When a solid is involved in a chemical reaction, either as reagent or a catalyst, the surface
area is the only accessible area for the reaction.

 As ratio of surface area to volume increases, surface phenomena come into play. For this
reason, measurement of surface area becomes much more important for small particles.
 BET
• Technique for the measurement of the specific surface area of materials.
• Applies to systems of multilayer adsorption, utilizes probing gases that do not chemically react with
material surfaces to quantify specific surface area.
• N₂ is the most commonly used. Thus, standard BET analysis conducted at the boiling temperature of
N₂ (77 K).
Test method is ISO 9277:2010
Determination of the specific surface area of solids by gas adsorption — BET method

Concept of BET method;

Assumptions of BET theory:

1. gas molecules physically adsorb on a solid in layers infinitely;

2. gas molecules only interact with adjacent layers; and
3. the Langmuir theory can be applied to each layer.
4. the enthalpy of adsorption for the first layer is constant and greater than the
second (and higher).
5. the enthalpy of adsorption for the second (and higher) layers is the same as the
enthalpy of liquefaction.
BET equation is

where P and Po are the equilibrium and the saturation pressure of adsorbate at the temperature of
adsorption, v is the adsorbed gas quantity, and vm is the monolayer adsorbed gas quantity. C is the BET
constant,

where E1 is the heat of adsorption for the first layer, and EL is heat of liquefaction.

Linear relationship is maintained only in the range of

0.05 < P/P0 < 0.35

N - Avogadro's number,
S - the adsorption cross section of the adsorbing species,
V - the molar volume of the adsorbate gas
a - mass of sample.
For the case of spherical, non-porous particles, the BET surface area is related to the particle
diameter (D) through

ABET is specific surface area

There are some limitations:

1. Particles must be totally separated from each others i.e. no agglomerates in the powder
used for BET test
2. Particles must be sphere or quasi-sphere. If not, the calculation will be inaccurate.
3. Some old BET instruments can not measure microporous material (diameter of pore less
than 2nm).
 REFERENCE
 https://en.wikipedia.org/wiki/BET_theory
 https://youtu.be/QQTb5JMQ4-s
 https://en.wikipedia.org/wiki/Particle-size_distribution
 https://www.academia.edu/5080328/Particle_size_ppt