Understanding Your Particle Size Analyzer Results

Interpreting Your Laser DiffractionParticle Size Analysis ResultsDecoding the Acronyms and Finding Insights

Ian Treviranusian.treviranus@horiba.comwww.horiba.com/us/particle

Outline

The Basics

Define Parameters

Choose Parameters

Interpret Results

The Workflow

The Problem

The BasicsParticle Distribution of Particles

The BasicsParticle Size Particle Size Distribution

The Basics

Which is the most meaningful size?

differentsize definitions

differentresults

The Basics

Which sizes can be measured?

The Basics

Laser DiffractionEquivalent Spherical Diameter

Dynamic Light ScatteringHydrodynamic Radius

Image AnalysisLengths, Widths, Equivalent Spherical

Acoustic SpectroscopyEquivalent Spherical Diameter

The BasicsLaser DiffractionAssumes hard, spherical shape model

q% = amount of each sizeby volume

The BasicsDynamic Light ScatteringAssumes hard, spherical shape model

Frequency % = amount of each sizeby volume

The BasicsImage AnalysisMeasures particle projection no shape assumption

UndersizePassingQ3

The BasicsAcoustic SpectroscopyAssumes hard, spherical shape model

Conclusions

Understand the dataA little goes a long way!

Know something about the particles in your sample

Particles have multiple dimensions, know which dimension your analyzer measures!

Outline

The Basics

Define Parameters

Choose Parameters

Interpret Results

Defining Parameters

Terms, Terms, and more Terms

Particle SizeMonomodal: One PeakBimodal: Two PeaksMultimodal: Multiple Peaks

Monodisperse: All particles have same sizePolydisperse: 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

Particle SizeFrequency% / q% / Amount of each size by volumep3 / Retained / Sph Vol%

Volume-based diameter Calculated from vol. distribution emphasizes coarse particles (larger volume)

Number-based diameter Calculated from number dist. (individual particles) emphasizes fine particles

Cumulative% on diameter % of distribution finer/coarser than specified size

Diameter on cumulative% Size at which a specified % of distribution is finer/coarser

Particle ShapeAcicular: Needle-shaped, rigidAngular: Edgy, hard anglesFibrous: Thread-like, non-rigidGranular/Blocky: Irregular-shaped, low aspect-ratioSpherical: Regular-shaped, unity aspect ratio

Aspect ratio: Breadth / length OR Length / breadthSphericity: How spherical is the particle?Roundness: How round is the particle?

Size Terminology

The most common designation is micrometers ormicrons. When very small, in colloid region, measured in nanometers, typically by ultra microscopes or by dynamic light scattering.

10-10 10-810-9 10-610-7 10-410-5 10-210-3 10-1 10-0

meternanometer

Angstrom(Å)

micrometer millimeterMicron or µm mnm mm

0.1µm 1.0µm 10µm 100µm

100 nm

Visible Particles: Lint, Dust, width of the ridges of fingertips.

Human Hair

Proteins, Viruses, and Macro-Molecules

Emulsions and ColloidsSuspensions and fine powdersSuspensions and fine powdersDust and free flowing powders

Relative Size

Central Values

Mean Medianand Mode

MeanWeighted AverageCenter of Gravity

Median50% Point

ModePeak of the distributionMost common value

Three spheres of diameters 1,2,3 units

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

What does “Mean” mean?

None of the answersare wrong they have just been calculated using different techniques

[ , ] .1 01 2 3

[ , ] .2 01 4 9

[ , ] .3 01 8 27

32 293

[ , ] .3 21 8 271 2 3

[ , ] .4 31 16 811 8 27

Many possible Mean values

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

D [4,3] =

D nD n

Monitoring the D[4,3] value in your specification will emphasize the detection of large particles

Volume-based Mean diameter

Median

D[4,3]

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

Central Values revisited

MeanWeighted AverageCenter of Gravity

Median50% Point

ModePeak of the distributionMost common value

D(v,0.9)D(v,0.1)

Size µmD(4,3) sensitive to large particles

D(v,0.5)median

D(v,1.0)Never use the D100!

10% of the particles are smaller than this diameter

90% of the particles are smaller than this diameter

half are larger than this diameterhalf are smaller than this diameter

Most Common Statistics

Standard Deviation

Normal (Gaussian) Distribution Curve

= distribution mean = standard deviation Exp = base of natural

logarithms

1 2Y = Exp [ - (x - )2

+1 STD DEV-1 STD DEV

+2 STD DEV-2 STD DEV

68.27%

95.45%

Distribution Width

Polydispersity Index (PI, PDI)

Span Geometric Std. Dev. Variance Etc…

Conclusions

Be familiar with the nomenclature

Many parameters can describe distributionD50, D10, D90 commonly usedSee Technical Note 156 in Download Center for more info

Which Mean do you mean?

Outline

The Basics

Define Parameters

Choose Parameters

Interpret Results

Choosing Parameters

Choosing good statistics

Statistics describing the distribution must…Tell us about our processBe relevantBe controlled wellBe reproducible!

Poor precision is the result of either a poor method or poor statistical choices

We can help! labinfo@horiba.com

Reproducibility!Prepare, measure, empty, repeat

What would be good reproducibility?Look at the accepted standards

ISO 13320COV < 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 µmNote: Must acquire at least 3 measurements from unique samplings

The Basis for Reliable Data

Unique, automatic feature in LA-950 softwareSee Technical Note 169 in Download Center

for instructions to use these features

Calculation Automation

Distribution Extremes

At a distance of a few standard deviations, non-instrumental errors can dominate

2 and 3 Standard Deviations

95% of the distribution is within 2 standard deviations from the Mean99.7% of the distribution is within 3

standard deviations from the mean

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

Better Method to Monitor Extremes

Instead of specifying the D95, D99, D99.99, D100, DMax

Specify the % of material greater than a certain size

Conclusions

Parameters should reflect product performanceBut 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 standardsISO 13320, USP <429> can provide guidance

Avoid monitoring the extremes whenever possibleBetter to use D(4,3) when you want spec. to be sensitive to presence of large particles

Outline

The Basics

Define Parameters

Choose Parameters

Interpret Results

Advanced Result Interpretation

GeneralMultiple ModesMultiple peaks can be better described individually

D50 D90D10

Laser DiffractionMultiple ScatteringWatch for finer “particles” appearing with increasing concentration

Multiple Scattering Example Zoom

0.00E+00

1.00E-01

2.00E-01

3.00E-01

4.00E-01

5.00E-01

6.00E-01

65 70 75

Detector Number (higher detector numbers for smaller particles)

1 Bottle2 Bottles3 Bottles4 Bottles5 Bottles6 Bottles7 Bottles8 Bottles9 Bottles10 Bottles

Multiple Scattering Example

0.00E+00

5.00E-01

1.00E+00

1.50E+00

2.00E+00

2.50E+00

45 50 55 60 65 70 75

Detector Number (higher detector numbers for smaller particles)

1 Bottle2 Bottles3 Bottles4 Bottles5 Bottles6 Bottles7 Bottles8 Bottles9 Bottles10 Bottles

Multiple Scattering

Laser DiffractionDispersing AgglomeratesWatch for no change in coarsest particles with changing energy

High = 3 barMid = 2 barLow = 1 bar

Laser DiffractionBreaking ParticlesWatch for finer particles being created with increasing energy

Conclusions

Look at the distribution graphSee the forest AND the trees

Precision != AccuracyVary measurement and calculation parameters

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

Understanding Your Particle Size Analyzer Results

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