Al-Qadisiyah University/College of

Engineering
Materials Engineering

Particle Size Analysis

Stage: Stage Four
2024
Subject: Nanotechnology and nanomaterials
Ruqayyah Kazim Hadi
Eng.saleh jawad
 Introduction

What is a particle? The simplest definition is a minute

portion of matter. Within the scope of this document
particles do not include subatomic particles such as
electrons, protons, neutrons, quarks, etc. Particles
measured by the techniques described here include
solids (powders), solids in liquids (suspensions), and
liquid/liquid emulsions. Not all particles exist as individ-
ual entities. They have a habit of sticking together to
form various kinds of clusters, or agglomerates. In
the field of particle technology, we typically define
agglomerates as a loose arrangement of larger
structures while aggregates are denser, harder to
disperse collectives.
 Most particles are not ideal spheres, but irregular in
shape. This creates a quandary when defining the
size of a particle using a single descriptive value. The
diameter of some kind of equivalent sphere is the only
available approach to describe particle size using a
single number. The International Union of Pure and
Applied Chemistry (IUPAC) definition1
of the equiva-
lent diameter of a non-spherical particle is equal to a
diameter of a spherical particle that exhibits identical
properties (e.g., aerodynamic, hydrodynamic, optical,
electrical) to that of the investigated non-spherical
particle. Most particle sizing techniques report results
as an equivalent spherical diameter (ESD).
 Particle size analysis, particle size measurement, or simply particle sizing, is the
collective name of the technical procedures, or laboratory techniques which
determines the size range, and/or the average, or mean size of the particles in a
powder or liquid sample.

Particle size analysis is part of particle science, and it is generally carried out in
particle technology laboratories.

The particle size measurement is typically achieved by means of devices, called

Particle Size Analyzers (PSA), which are based on different technologies, such as high
definition image processing, analysis of Brownian motion, gravitational settling of
the particle and light scattering (Rayleigh and Mie scattering) of the particles.

The particle size can have considerable importance in a number of industries

including the chemical, food, mining, forestry, agriculture, cosmetics,
pharmaceutical, energy, and aggregate industries.
01 03 04
Many numerical descriptors can be used to describe
the properties of particle size distributions. The term
average particle size is not typically used in this field
of technology. The mean is a calculated central point
in the distribution.
PARTICLE CHARACTERIZATION TECHNIQUES
—
There are many analytical techniques available for
particle size analysis. Various techniques have different
capabilities and dynamic range as well as assorted
strengths and weaknesses. Before choosing an analytical
technique, the user should first define what is required
by the instrument and how the data will be used. After
this is determined it can still be challenging to review
all possible techniques and select the best option for
a given requirement. This document is intended to
help scientists new to particle size analysis understand
some of the available techniques and how to select
the proper technique for their samples.
Questions to be considered when choosing a particle
size analyzer include:
• What is the size range of interest?
• Is the particle size distribution the only
result required?
• Does the surface charge matter?
• Is it helpful to know the concentration
of the particles?
• How much automation is required?
• What format should the results be in?
– Number distribution? Volume distribution?
After these questions are understood the technique
and then specific instrument selections will become
easier.
 The correlator takes this information and determines
the diffusion coefficient of the particles in the sample.
The diffusion coefficient is then used to calculate the
particle size using the Stokes-Einstein equation:
D = kT/6π ŋR
Where:
D = Diffusion coefficient
R = Particle radius
k = Boltzmann’s constant
T = Temperature Kelvin
ŋ= Shear viscosity of the solvent
 PARTICLE COUNTING
Coulter Counter
The first particle counter/size analyzer is known as
electrical sensing zone or the Coulter counter. With
this technique particles must be suspended in an
electrolytic solution. As particles flow through an
aperture a change in impedance is proportional to
the volume of the particle, Figure 11. The physics
of the aperture geometry and electronics limits the
dynamic range to an approximately 30:1 ratio, for
example a 140 µm aperture can measure from
2.8 – 84 µm.
While the Coulter counter is still used in hematology,
it is now seldom used for general particle size
analysis
due to the limited dynamic range and practical
difficul-
ties with particles clogging the orifices.
LABORATORY VS. ONLINE ANALYSIS

Most particle size analysis measurements are per-

formed in the laboratory. Some, but not all, particle
sizing techniques can and have been adapted to
the process environment for online measurements.
Online image analysis can be used for both powders
and liquids. DLS with automatic dilution has been
used to monitor size reduction operations such as
homogenization. Laser diffraction has been more
successfully adapted to free-flowing powders than
suspensions due to the challenges in keeping optical
windows clean. Liquid particle counters are often used
online for contamination control of pure DI water
and chemical applications. Online SPOS systems
are used in fabs around the world to monitor large
particle counts (LPCs) in CMP slurries
 RESULT COMPARISONS
µm emulsion sample was analyzed using several techniques including
DLS, laser diffraction, and SPOS.
The size of 1 µm was chosen since this lies within the dynamic range of all
three technologies. The DLS results using both the Gaussian unimodal
and Nicomp multi-modal algorithm.The Gaussian result indicates a high
Chi Squared value
of 744.1, strongly suggesting multiple peaks and that
the multi-modal algorithm result should be used for
this data. The multi-modal algorithm result reports a
first peak at 950 nm (0.95 µm) and a larger peak at
10433.4 (10.43 µm).
 The same sample was analyzed using the AccuSizer
AD SPOS system. This instrument uses exponential
dilution to reduce the concentration to the optimum
level to avoid coincidence error (more than one particle
at a time in the measurement zone). The LE400 sensor
has a dynamic range of 0.5 – 400 µm. The counts/mL,
or number distribution, is shown in Figure 17 where
the main peak is centered near 1 µm.

The result was then converted

to the volume distribution.

The conversion from number to volume distributions

with the AccuSizer system is accurate and justifiable.
Now the first peak remains at 1 µm and a larger peak
is reported at 6 µm.
 The volume distribution shows the 1 um main peak but also shows
how larger droplets make up some of the volume.
The same sample was analyzed using a Horiba LA-960 laser
diffraction system
This study highlights both the similarities and differences between
results generated by several particle size analysis techniques. None of
the results match each other perfectly. That is the real-world
situation when comparing results analyzed using different
technologies. Each technique has advantages and disadvantages.
DLS is the most popular technique for sub-micron samples, but data
interpretation can become challenging and not all multi-modal
algorithms are created equally. The SPOS technique provides high-
accuracy, high-resolution results and has the best sensitivity to tails
of distributions. But SPOS is not well suited for powders or sprays.
 referencesrefer
1- McNaught, A. and Wilkinson, A., Compendium of Chemical
Terminology, Oxford, 1997
2- Entegris Technical Note – Number of Particles Analyzed

3- From ISO 13320-1, Particle size analysis – Laser Diffraction

Methods, Part 1: General Principles
THANK'S FOR LARANA, INC.

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