Interpreting Your Laser Diffraction

Particle Size Analysis Results

Decoding the Acronyms and Finding Insights

Ian Treviranus
ian.treviranus@horiba.com
www.horiba.com/us/particle

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 Outline

The Basics

Define Parameters

Choose Parameters

Interpret Results

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 The Workflow

+ +

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 The Problem

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 The Basics
Particle Distribution of Particles

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 The Basics
Particle Size Particle Size Distribution

4 µm

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 The Basics

Which is the most meaningful size?

different different
size definitions results

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 The Basics

Which sizes can be measured?

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 The Basics

Laser Diffraction
Equivalent Spherical Diameter

Dynamic Light Scattering

Hydrodynamic Radius

Image Analysis
Lengths, Widths, Equivalent Spherical

Acoustic Spectroscopy
Equivalent Spherical Diameter

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 The Basics
Laser Diffraction
Assumes hard, spherical shape model

q% = amount
of each size
by volume

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 The Basics
Dynamic Light Scattering
Assumes hard, spherical shape model

Frequency %
= amount
of each size
by volume

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 The Basics
Image Analysis
Measures particle projection  no shape assumption

Undersize
Passing
Q3

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 The Basics
Acoustic Spectroscopy
Assumes hard, spherical shape model

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 Poll!

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 Conclusions

 Understand the data

A little goes a long way!

 Know something about the particles

in your sample

 Particles have multiple dimensions,

know which dimension your analyzer
measures!

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 Outline

The Basics

Define Parameters

Choose Parameters

Interpret Results

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 Defining Parameters

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 Terms, Terms, and more Terms

Particle Size
Monomodal: One Peak
Bimodal: Two Peaks
Multimodal: Multiple Peaks

Monodisperse: All particles have same size

Polydisperse: Particles have many sizes

Volume diameter: Diameter of a sphere having the same

volume as the particle
Surface diameter: Diameter of a sphere having the same
surface as the particle

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 Terms, Terms, and more Terms
Particle Size
Frequency% / q% /
p3 / Retained / Sph Vol%
Volume-based diameter
Number-based diameter
Cumulative% on diameter
Diameter on cumulative%
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Amount of each size by volume
Calculated from vol. distribution
emphasizes coarse particles
(larger volume)
Calculated from number dist.
(individual particles)
emphasizes fine particles
% of distribution finer/coarser
than specified size
Size at which a specified % of
distribution is finer/coarser
 Terms, Terms, and more Terms

Particle Shape
Acicular: Needle-shaped, rigid
Angular: Edgy, hard angles
Fibrous: Thread-like, non-rigid
Granular/Blocky: Irregular-shaped, low aspect-ratio
Spherical: Regular-shaped, unity aspect ratio

Aspect ratio: Breadth / length OR Length / breadth

Sphericity: How spherical is the particle?
Roundness: How round is the particle?

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 Poll!

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 Size Terminology
0.1µm 1.0µm 10µm 100µm

10-10 10-9 10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1 10-0
100 nm

nanometer micrometer millimeter meter

nm Micron or µm mm m

Angstrom
(Å)

The most common designation is micrometers or

microns. When very small, in colloid region,
measured in nanometers, typically by ultra
microscopes or by dynamic light scattering.

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 Relative Size

Human Hair

Visible Particles: Lint, Dust, width

of the ridges of fingertips.
Dust and free flowing powders
Suspensions and fine powders
Suspensions and fine powders
Emulsions and Colloids
Proteins, Viruses, and Macro-
Molecules

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 Poll!

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 Central Values

Mean
Weighted Average Mean
Center of Gravity Median
and
Mode
Median
50% Point

Mode
Peak of the distribution
Most common value

Size

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 What does “Mean” mean?
Three spheres of diameters 1,2,3 units

1
2
3

What is the average size of these spheres?

Average size = (1+2+3) ÷ 3 =2.00
This is called the D[1,0] - the number mean

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 Many possible Mean values
1 2  3
X nl  D[1,0]   2.00
3
1 4  9 None of the answers
X ns  D[ 2,0]   2.16
3 are wrong they have just
been calculated using
1  8  27 different techniques
X nv  D[ 3,0]  3  2.29
3

1  8  27
X sv  D[ 3,2]   2.57
1 2  3

1  16  81
X vm  D[ 4,3]   2.72
1  8  27

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 Volume-based Mean diameter
D[4,3] which is often referred to as the Volume Mean Diameter [ VMD ]

D [4,3] =
D n 4
i i

D n 3
i i

Monitoring the D[4,3] value in your specification

will emphasize the detection of large particles

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 Central Values revisited

Mean
Weighted Average
Mode
Center of Gravity
Median

Mean Median
50% Point
D[4,3]

Mode
Peak of the distribution
Most common value

Size

Remember: D[4,3] is sensitive to large particles

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 Most Common Statistics
half are smaller than this diameter half are larger than this diameter
D(v,0.5)
median

10% of the particles are 90% of the particles are

smaller than this diameter smaller than this diameter
D(v,0.1) D(v,0.9)
D(v,1.0)
Never use
the D100!
Size µm
D(4,3) sensitive to large particles

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 Standard Deviation

 Normal (Gaussian)
Distribution Curve
-1 STD DEV +1 STD DEV   = distribution mean
68.27%
  = standard deviation
 Exp = base of natural
logarithms

-2 STD DEV +2 STD DEV

95.45%

Mean

1 - (x - )2
Y=  2 Exp [ ]
22
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 Distribution Width

 Polydispersity Index
(PI, PDI)
 Span
 Geometric Std. Dev.
 Variance
 Etc…

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 Poll!

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 Conclusions

 Be familiar with the nomenclature

 Many parameters can describe

distribution
D50, D10, D90 commonly used
See Technical Note 156 in Download Center for more info

 Which Mean do you mean?

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 Outline

The Basics

Define Parameters

Choose Parameters

Interpret Results

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 Choosing Parameters

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 Choosing good statistics

Statistics describing the distribution must…

Tell us about our process
Be relevant
Be controlled well
Be reproducible!

Poor precision is the result of either a poor

method or poor statistical choices
We can help!
labinfo@horiba.com

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 The Basis for Reliable Data
Reproducibility!
Prepare, measure, empty, repeat

What would be good reproducibility?

Look at the accepted standards

ISO 13320
COV < 3% at Median (D50) COV = 100 * (StDev / Mean)
COV < 5% at D10 and D90

USP <429>
COV < 10% at Median (D50)
COV < 15% at D10 and D90

Note: All limits double when D50 < 10 µm

Note: Must acquire at least 3 measurements from unique samplings
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 Calculation Automation

Unique, automatic feature in LA-950 software

See Technical Note 169 in Download Center
for instructions to use these features

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 Distribution Extremes

At a distance of a few standard

deviations, non-instrumental errors can
dominate

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 2 and 3 Standard Deviations

95% of the distribution is within 2 standard

deviations from the Mean
99.7% of the distribution is within 3
standard
deviations
from the mean

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 Reproducibility at the Extremes

If we want the same level of reproducibility at

the D99 value as the D50, we need to
analyze similar amounts of material in the
D99 histogram band

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 Better Method to Monitor Extremes
Instead of specifying the D95, D99,
D99.99, D100, DMax

Specify the % of material greater than a

certain size

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 Poll!

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 Conclusions
 Parameters should reflect product
performance
But don’t make your life more difficult than it needs to be!
See Webinar TR007 Setting Size Specifications and
Technical Note 161 for more information

 Look to appropriate standards

ISO 13320, USP <429> can provide guidance

 Avoid monitoring the extremes

whenever possible
Better to use D(4,3) when you want spec. to be
sensitive to presence of large particles

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 Outline

The Basics

Define Parameters

Choose Parameters

Interpret Results

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 Advanced Result Interpretation

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 General
Multiple Modes
Multiple peaks can be better described individually

D10 D50 D90

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 Laser Diffraction
Multiple Scattering
Watch for finer “particles” appearing with increasing concentration

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 Multiple Scattering
Multiple Scattering Example

2.50E+00
1 Bottle
2.00E+00 2 Bottles
3 Bottles

Light Intensity
4 Bottles
1.50E+00
5 Bottles
6 Bottles
1.00E+00
7 Bottles
8 Bottles
5.00E-01 9 Bottles
10 Bottles
0.00E+00
45 50 55 60 65 70 75
Detector Number (higher detector numbers for smaller particles)

Multiple Scattering Example Zoom

6.00E-01
1 Bottle
5.00E-01
2 Bottles
3 Bottles
4.00E-01
Light Intensity

4 Bottles
5 Bottles
3.00E-01
6 Bottles
7 Bottles
2.00E-01
8 Bottles

1.00E-01 9 Bottles
10 Bottles
0.00E+00
65 70 75
Detector Number (higher detector numbers for smaller particles)

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 Laser Diffraction
Dispersing Agglomerates
Watch for no change in coarsest particles with changing energy

2 bar

1 bar

3 bar

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 Laser Diffraction
Breaking Particles
Watch for finer particles being created with increasing energy

High = 3 bar
Mid = 2 bar
Low = 1 bar

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 Conclusions

Look at the distribution graph

See the forest AND the trees

Precision != Accuracy
Vary measurement and calculation parameters

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 For More Details

Visit www.horiba.com/us/particle

Contact us directly at labinfo@horiba.com

Visit the Download Center to find this recorded

presentation and many more on other topics

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