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Particle Size Analysis by Laser Diffraction

Introduction
The underlying assumption in the design of laser
diffraction instruments is that the scattered light
pattern formed at the detector is a summation of
the scattering pattern produced by each particle
that is being sampled. Deconvolution of the
resultant pattern generates information about the
scattering pattern produced by each particle and,
upon inversion, information about the size of the
particle.

3. The scattering pattern at the detectors is the


sum of the individual scattering patterns
generated by each particle.
Experimental
Prior to analysis, the dispersion cell is filled with
clean, deionised water and left to allow thermal
equilibrium to take place. The instrument
automatically aligns so that the incident path of
the laser is aligned with the optical arrays. The
cleanliness of the system is then checked, and a
background is taken. By comparing the signal
intensity of the system without a sample present,
to the intensity with a sample, the obscuration of
the laser beam may be calculated, giving some
idea of the material concentration in the dispersal
cell. Too high a concentration results in multiple
scattering, too low and the signal strength is
inadequate to register at the detectors. Figure 2
below illustrates a comparison between the
signals obtained from an empty system (red), with
that from a particle sample (green). The
background signal should always be lower than
your sample signal!
Data Graph - Light Scattering

800

Figure 1: Light scattering patterns observed for


polystyrene latex particles

Light Energy

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In essence, each particle scatter pattern is


matched to a theoretical pattern using
comprehensive mathematical solution to the
scattering of incident light by spherical particles;
the Mie Theory. This theory indicates the
necessity for a precise knowledge of the real and
imaginary components of the refractive index of
the material being analysed, to determine particle
size and particle size distribution. When a good fit
is obtained, then we know all of the relevant
information in order to deconvolute the Mie
pattern into meaningful particle size information.
All laser diffraction instruments rely on three basic
tenets:
1. The particles scattering the light are spherical in
nature.
2. There is little to no interaction between the light
scattered from different particles.

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0
1 3 5 7 9

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Detector Number

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Figure 2: Background and sample scattering data


Suitable dispersion procedures should be followed
to ensure that the powder is dispersed and
minimum agglomeration has taken place. Care
must also be taken to ensure that the dispersal
cell contains no air bubbles or that particle
fracture is not occurring as the instrument is not
capable of distinguishing between agglomerates,
air bubbles or primary particles.
Sonification is an option to aid particle dispersion
although again, care must be taken to ensure the
correct intensity and duration of sonification to
avoid primary particle breakage.
The particle size distribution will depend on the
optical model used to calculate it! The real and

AN003 Particle size analysis by laser diffraction rev 0.doc

Data Graph - Light Scattering

Light Energy

imaginary components of the refractive index are


a vital part of the particle characterisation
equation. In the case of an unknown particle
refractive index (if a literature value is
unavailable), the optical properties may be
derived by varying the input values and comparing
the resultant scatter pattern with the measured
data until a good fit is obtained.

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0

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Detector Number
Fit data(weighted)
Imaginary part of refractive index = 0.1, 20 February 2004 15:32:21

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Figure 5: Imaginary RI component = 0.1


Data Graph - Light Scattering

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Volume (%)

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Detector Number
Fit data(weighted)
Imaginary part of refractive index = 1.0, 20 February 2004 15:32:21

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Figure 6: Imaginary RI component = 1.0

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6
4
2
0
0.01

0.1

1
Particle Size (m)

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Imaginary part of refractive index = 0.01


Imaginary part of refractive index = 0.1
Imaginary part of refractive index = 1.0

Figure 3: Size distributions using varying


imaginary RI values
If we look at the theoretical scatter pattern
compared with the measured data, we get an
instant idea of the goodness of fit. Figures 4, 5
and 6 illustrate the comparison when using an
imaginary refractive index of 0.01. 0.1 and 1.0
respectively.
Data Graph - Light Scattering

60
Light Energy

30
Light Energy

In figure 3 below, we see the difference the


imaginary part of the refractive index makes to the
resulting size distribution. The question is which
value gives the correct distribution?

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40

We clearly see the evolution in scatter pattern as


the actual data starts to approach the theoretical,
until at an imaginary RI component of 1, the
patterns coincide. At this point, we can say that
this scatter pattern is the most correct, and in this
case, the true size distribution will be the blue line
in figure 3.
Conclusions
1. Sample preparation is important; the
instrument must be aligned and clean.
2. Laser diffraction particle sizing requires both
the real and imaginary components of the
particle under analysis
3. By adjusting RI values manually, the scatter
pattern may be manipulated until actual and
theoretical are congruent. At this point, we
may say our input RI is correct, and the
resultant size distribution is representative of
the system under analysis.

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1 3 5 7 9 11
14
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Detector Number
Fit data(weighted)
Imaginary part of refractive index = 0.01, 20 February 2004 15:32:21

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Figure 4: Imaginary RI component = 0.01

AN003 Particle size analysis by laser diffraction rev 0.doc

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