Size measurement Flashcards

1
Q

Challenges in measuring particle size

A

1) Cannot describe a 3D object with just one number
- Assumes particle is a sphere, which may not be true
2) Different sizing methods may give different size information

Overall: Sizing methods involve a lot of derivation & estimation
- Data interpretation and validation of accuracy & reliability of results can be difficult

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2
Q

Equivalent sphere theory

A

Determines diameter of a sphere that has the same weight as a particle of a particular weight
- Can be used to gauge if particle becomes larger/smaller

Weight of sphere = 4/3 π r^3 p

  • r = Radius of sphere
  • p = Density
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3
Q

List of particle sizing methods & particle size that can be measured

A

1) Scales (vernier, micrometer): > 5 mm (larger particles)
2) Sieves: > 10 µm
3) Microscopy (image analysis): 5 µm - 5 mm
4) Laser diffraction: 5 µm - 5 mm
5) Laser scattering: 0.001 µm - 5 µm
6) Sedimentation: 0.05 µm – 150 µm
7) Scanning electron microscope (SEM): nm - µm
8) Atomic force microscope (AFM): nm - µm

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4
Q

Microscopy - How it works

A

Particle size depends on what is measured:

1) Maximum particle length as diameter
2) Minimum diameter
3) Other diameters (e.g. Feret’s diameter)
4) Minimum length
5) Volume
6) Surface area

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5
Q

Microscopy - Types of diameter measurements

A

1) Feret’s diameter
- Greatest distance possible between any 2 points along boundary of region of interest OR
- Distance between 2 vertical lines tangent to ends of particle

2) Martin’s diameter
- Length of horizontal line that appears to divide particle in half

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6
Q

Microscopy - No. of images to examine

A

National Bureau of Standards (NBS) recommendation: Min 10,000 images for statistical validity

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7
Q

Microscopy - Advantages

A

1) Direct visual examination
- Can differentiate between individual particles & agglomerates
2) Relatively cheap

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8
Q

Microscopy - Disadvantages

A

1) Operator dependent; Manual method
- Prone to bias
- May have non-representation –> fewer particles examined (but impact might not be as large if only smaller particles missed)
2) Sample preparation requires skill & can be laborious & slow
3) Only provides 2D image
- Particles tend to be oriented in position with lowest centre of gravity –> tend to measure maximum diameter of particle

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9
Q

Sieves - How it works

A

Longer measurement time –> smaller particle size

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10
Q

Sieves - Advantages

A

1) Economical & robust technique for larger particles

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11
Q

Sieves - Disadvantages

A

1) Low resolution method

2) Usually only 4-8 size fractions provided

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12
Q

Sieves - Application

A

1) May be used for quality control

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13
Q

Air jet sieve - How it works

A

1) Weighed material placed on sieve of certain aperture size (may be microsieve)
2) Jet of air blown upwards –> particles blown as well
- Creates pressure in chamber
- Separates particles
3) As air escapes –> particles pulled out with air
- Only particles of size ≤ aperture size may be pulled out
4) Remaining particles weighed
5) Calculate cumulative weight %
6) Repeat with sieves of other aperture size

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14
Q

Air jet sieve - Determining particle size

A

Plot graph of cumulative weight % against sieve equivalent diameter

Mass median diameter = D50 = Sieve equivalent diameter when cumulative weight % = 50%

Span (Size distribution) = (D90 - D10) / D50

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15
Q

Air jet sieve - Application

A

Fine particles < 200 µm (35 - 200 µm)

- Such particles tend to form agglomerates that are difficult to break down and sieve with normal sieve

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16
Q

Electrozone sensing - How it works

A

Particles dispersed in electrolyte as suspension
Liquid pulled into tube through an orifice
As particles pass through orifice –> block orifice to some extent –> resistance occurs –> decrease in conductivity
Particle size is proportionate to resistance
- Larger particles –> greater resistance
Particle size determined by comparing to reference size calibrator

17
Q

Electrozone sensing - Advantages

A

Unaffected by optical properties, densities, shape, colour of particles

18
Q

Electrozone sensing - Limitations

A

1) Calibration standards required
- Expensive
- Can change in distilled water and electrolyte
2) Particle size should not be too large/small
- Large –> sediment quickly
- Not easy to measure particles < 2µm
- Particle size should be 2 - 5 µm
3) Porous & dense particles should not be used
- Porous –> different displacement of water
- Dense –> tend to settle

19
Q

Electrozone sensing - Applications

A

1) Originally used for sizing blood cells
2) Particles sized should be:
- 2 - 5 µm
- Non-porous, non-conducting, insoluble

20
Q

Laser diffraction / Low Angle Light Scattering (LALLS) - How it works

A

When light passes through particle –> scattering/diffraction of light occurs
Light scattering pattern measured by diodes
Higher angle scatter –> smaller particle
Volume distribution can be generated, equal to weight distribution where density is constant

21
Q

Laser diffraction / Low Angle Light Scattering (LALLS) - Advantage

A

1) Efficient, economic
2) Wide dynamic range, very flexible
3) Possible to measure dry powder, spray or particles in air/liquid
4) Rapid
5) Repeatable, with high resolution
6) No need for calibration against against a standard but equipment performance can be easily verified
7) Only small amount of particles needed to carry out measurement

22
Q

Laser diffraction / Low Angle Light Scattering (LALLS) - Application

A

1) Used for wide range of particle sizing

2) Method of choice for particle characterization & QC

23
Q

Light Scattering - How it works

A

Based on Brownian motion
- Applicable to particles < 2 - 3µm
Smaller particles –> faster movement/diffusion
Pace can be detected by analyzing the time dependency of light intensity fluctuations scattered from particles when they are illuminated
- Longer light if reflected back –> moving at slower speed –> larger particle

24
Q

Photon correlation spectroscopy - How it works

A

Shine light at particles –> light is scattered & detected –> auto-correlation to determine size of particles

25
Q

Photon correlation spectroscopy - Application

A

Used to measure size of particles 0.01 - 5 µm