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03 Part Characterisation Lecture

The document discusses particle characterization in chemical manufacturing, focusing on the various uses of solids as feed, products, and process additives. It outlines methods for measuring particle size distribution (PSD), including sieve analysis, microscopy, laser diffraction, and dynamic light scattering, while explaining key concepts such as equivalent diameters and statistical diameters. Additionally, it emphasizes the importance of particle properties like shape, density, and flowability in various unit operations.

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0% found this document useful (0 votes)
7 views43 pages

03 Part Characterisation Lecture

The document discusses particle characterization in chemical manufacturing, focusing on the various uses of solids as feed, products, and process additives. It outlines methods for measuring particle size distribution (PSD), including sieve analysis, microscopy, laser diffraction, and dynamic light scattering, while explaining key concepts such as equivalent diameters and statistical diameters. Additionally, it emphasizes the importance of particle properties like shape, density, and flowability in various unit operations.

Uploaded by

u21589969
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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CPA 410 Particle

technology
3. Particle Characterisation

BJ du Plessis
March 2024
Chemical manufacturing processes use solids, amongst others, as:

Feed - Coal, Wood chips, Plastic pellets, Food, etc.

Product - Fertiliser, washing powder, died fruit, table salt, cement, etc.

Process additives - Activated carbon, Chemical salts, Brewers yeast etc.

Catalyst or Column packing


A number of unit operations exist where particles are Solids characteristics
used, amongst others:
Physical properties
Packed beds Particle Size
Settling/Thickening Particle shape
Fluidisation Velocities
Filtration Surface properties
Cyclones Flowability
Dryers Density and bulk density
Comminution Mechanical properties
Agglomeration Charge properties
Screening
Pneumatic transport Chemical composition
Powder mixing
Leaching
Ion exchange/Adsorption
What is the size of these objects?
1 mm
2 mm

1 mm
3 mm

4 mm
1 mm

1 mm
1 mm

1 mm

1 mm
Single Particle

Equivalent diameters in terms of sphere


Equivalent Volume diameter (dV) SA sphere = D2
i.e. what is diameter of sphere that has same volume as particle? Vol of sphere = D3/6
Equivalent Surface Area diameter (dSA)
i.e. what is the diameter of a sphere that has the same surface area of the particle?

Example 3 13 ×6
VP = 13 = dv3/6 𝑑𝑣 = = 1.241 mm
𝜋
1 mm

1 mm

6 × (1 × 1)
SAP = 6 × (1×1) = dSA 2 𝑑𝑆𝐴 = = 1.382 𝑚𝑚
1 mm 𝜋
Single Particle

Equivalent Surface volume diameter - dSV (Sauter diameter ds)

i.e. what is the diameter of a sphere with the surface area to volume ratio of the particle

 d sv3 Vp 6V p
6 =  d sv =
d 2
sv Ap Ap

Example

1 mm
6 ×1
𝑑𝑆𝑉 = = 1 𝑚𝑚
6
1 mm

1 mm
Which diameter depends on what it will be used for

Surface diameter
Adsorption and reaction engineering, equivalent surface exposure area is important.

Volume diameter
Solids holdup in a packed bed or in the calculation of buoyancy forces of the particles.

Sauter's diameter
Areas where the specific surface area is of most interest. Such areas include catalysis, settling, etc.
Single Particle

Sphericity is a measure of how closely the shape of an object resembles that of a perfect sphere.

The sphericity  of a particle is the ratio of the surface area of a sphere with the same volume as the
given particle to the surface area of the particle.
2ൗ
6𝑉𝑝 3
𝜋
𝑆𝐴 𝑜𝑓 𝑠𝑝ℎ𝑒𝑟𝑒 𝑤𝑖𝑡ℎ 𝑠𝑎𝑚𝑒 𝑣𝑜𝑙 𝑎𝑠 𝑝𝑎𝑟𝑖𝑐𝑙𝑒 𝜋𝑑𝑣2 𝜋
𝜓= = =
𝑆𝐴 𝑜𝑓 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒 𝑆𝐴𝑝 𝑆𝐴𝑝

Example
3 13 ×6
𝑑𝑣 = = 1.241 mm
1 mm 𝜋
VP = 13 = dv3/6

1 mm 𝜋 (1.241)2
SAP = 6 × (1×1) = dSA 2
𝜓= = 0.806
6
1 mm
Single Particle

Aspect ratio

ISO 9276-6
Particle size distribution (PSD)

What size are these particles?

We need 1 value to describe the average particle size


Measuring
Particle size distribution (PSD)
Sieve analysis

700

600

500

400

300

200

Pan
Measuring
Particle size distribution (PSD)
British fine Aperture
US Tyler Aperture (µm) Mesh (µm)
16 991 14 1204
20 833 16 1003
24 701 18 853
28 589 22 699
32 495 25 600
35 417 30 500 Sizes vary by a factor of √2
42 351 36 422
48 295 44 353
60 248 52 295
65 208 60 251
80 175 72 211
100 147 85 178
115 124 100 152
150 104 120 124
170 88 150 104
200 74 170 89
230 61 200 76
270 53 240 66
325 43 300 53
Particle size distribution (PSD)
Example 1
Mass
Size (µm)
(gram)
800 - 700 0
700 - 600 5 700
600 - 500 50
500 - 400 100 600
400 - 300 50
300 - 200 15 500
200 - 0 0
400

300

200

Pan
Example 1
50
Avg size Mass Fraction
Size (mm)
(mm) (gram) (fi)
800 - 700 750 0 0 40
700 - 600 650 5 2.3
600 - 500 550 50 22.7 30
500 - 400 450 100 45.5
400 - 300 350 50 22.7 20
300 - 200 250 15 6.8
200 - 100 150 0 0
10
Total 220 100

0
0 100 200 300 400 500 600 700 800
Example 1 𝑖

𝐹𝑖 = ෍ 𝑓𝑖
0
Mass Fraction Cum Fraction > dP 100
Size (µm) 90
(gram) (fi) (Fi) 80
800 - 700 0 0 0 70
700 - 600 5 2.3 2.3 60 How much
600 - 500 50 22.7 25.0 50 is bigger
40 than 500
500 - 400 100 45.5 70.5 30
400 - 300 50 22.7 93.2 20
300 - 200 15 6.8 100.0 10
0
200 - 0 0 0 100.0
Total 220 100
Example 1

Avg size Mass Fraction Cum Frac < dP 100.0


Size (mm)
(mm) (gram) (fi) (Fi)
800 - 700 750 0 0 100.0 75.0
700 - 600 650 5 2.3 100.0 How much
600 - 500 550 50 22.7 97.7 is smaller
50.0 than 500

Fi
500 - 400 450 100 45.5 75.0
400 - 300 350 50 22.7 29.5
25.0
300 - 200 250 15 6.8 6.8
200 - 100 150 0 0 0
Total 220 100 0.0
0 500 1000
dP
Example 1

100

100 90

90 80

80 70

70 60

60 50

50 40

40 30

30 20
20 10
10 0
0
Measuring
Particle size distribution (PSD)
Microscopy (or image analysis)
Measuring
Particle size distribution (PSD)
Example 2
35
Avg. size Number Number
Size (mm)
(mm) Particles fraction 30
800 - 700 750 0 0
700 - 600 650 250 0.5 25
600 - 500 550 4250 8.5
500 - 400 450 15500 31 20
400 - 300 350 16500 33
300 - 200 250 13500 27 15
200 - 100 150 0 0
Total 50000 100.0 10

0
0 100 200 300 400 500 600 700 800
Data display
Frequency distribution curve Cumulative distribution curve

50 120
45
40 100
35 80
30
25 60

Fi
fi

20
40
15
10 20
5
0 0
0 500 1000 0 200 400 600 800
dP dP
Conversion from number to mass distribution

𝜋 3 𝑉 = 𝑘𝑉 𝐷 3
𝑉= 𝐷 𝑉 = 1 𝐷3
6

𝑉𝑜𝑙 𝑜𝑓 1 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒 = 𝑘𝑉 𝑑𝑖3

𝑚𝑖 = 𝑛𝑖 𝜌𝑠 𝑘𝑉 𝑑𝑖3
Conversion from number to mass distribution 𝑚𝑖 = 𝑛𝑖 𝜌𝑠 𝑘𝑉 𝑑𝑖3

Avg size (mm) Num frac (ni) mi fi


750 0 0 0.0
650 0.5 0.5×(650)3 SkV = 137312500SkV 2.2
550 8.5 1414187500SkV 22.8
450 31 2824875000SkV 45.5
350 33 1414875000SkV 22.8
250 27 421875000SkV 6.8
150 0 0 0.0
Total 6213125000SkV
𝑖

𝐹𝑖 = ෍ 𝑓𝑖 = න 𝑓𝑖 𝑑𝑃
0

Avg size
(mm) fi Fi > d P
750 0
650 2.3
550 25.0
𝑑𝐹
𝑓𝑖 = 450 70.5
𝑑𝑑𝑃 350 93.2
250 100.0
150 100.0
Measuring
Particle size distribution (PSD)

Laser diffraction

Volume distribution
Measuring
Particle size distribution (PSD)
Dynamic light scattering
Measuring
Particle size distribution (PSD)
Coulter counter
Measuring
Particle size distribution (PSD)

Sedigraph (Terminal settling velocity of particles)


Measuring
Particle size distribution (PSD)

Permeability meter (Flow through a packed bed of particles)


What does “Mean” mean?

1mm 2mm 3mm


𝑁𝑢𝑚𝑏𝑒𝑟 𝑚𝑒𝑎𝑛 (𝑎𝑣𝑒𝑟𝑎𝑔𝑒) = 2.00

𝑆𝑢𝑟𝑓𝑎𝑐𝑒 𝑎𝑟𝑒𝑎 𝑚𝑒𝑎𝑛 = 2.16

𝑉𝑜𝑙𝑢𝑚𝑒 𝑚𝑒𝑎𝑛 = 2.29


Particle size distribution (PSD)
Statistical diameters

100

75

Median  d50 50

Fi
25

0
0 500 1000
dP

The mass mean particle size (Average) dm = (fidi)


Example 1

100 100
90 90
80 80
70 70
60 60
50 50
40 40
30 30
20 20
10
10
0
0
100.0
d80 90.0
80.0
70.0
60.0
50.0
Fi

40.0
30.0
d20
20.0
10.0
0.0
100 1000
dP
Equivalent diameter

Equivalent volume diameter


What is the diameter of a particle, such that the total number of particles
and the total volume is the same as in original sample

𝑉 = ෍ 𝜌𝑠 𝑘𝑑𝑖3 𝑛𝑖
Original Sample

𝑉 = ෍ 𝜌𝑠 𝑘𝑑𝑣3 𝑛 𝑇

Equivalent Sample
෍ 𝜌𝑠 𝑘𝑑𝑣3 𝑛𝑖 = ෍ 𝜌𝑠 𝑘𝑑𝑖3 𝑛𝑖

𝜌𝑠 𝑘𝑑𝑣3 ෍ 𝑛𝑖 = 𝜌𝑠 𝑘 ෍ 𝑑𝑖3 𝑛𝑖

3
3
σ 𝑛 𝑑
𝑖 𝑖 Number distribution
𝑑𝑣 =
σ 𝑛𝑖
Mass distribution
𝑓𝑖 𝑚 𝑇
mi = fimT= s ni k di3 𝑛𝑖 =
𝜌𝑠 𝑘𝑑𝑖3

𝑓 𝑚
σ 𝑖 𝑇3 𝑑𝑖3 𝑚𝑇
σ 𝑓𝑖
σ 𝑛𝑖 𝑑𝑖3 𝜌𝑠 𝑘𝑑𝑖 𝜌𝑠 𝑘 σ 𝑓𝑖
𝑑𝑣3 = σ 𝑛𝑖
= 𝑓 𝑚 = 𝑚𝑇 𝑓𝑖 = 𝑓
σ 𝑖 𝑇3 σ σ 3𝑖
𝜌𝑠 𝑘𝑑𝑖 𝜌 𝑠 𝑘 𝑑3 𝑑𝑖
𝑖
Number Mass/Volume

σ 𝑛𝑖 𝑑𝑖3 1
= =
dsv Sauter
σ 𝑛𝑖 𝑑𝑖2 σ 𝑓𝑖ൗ𝑑
𝑖

σ 𝑓𝑖ൗ𝑑
σ 𝑛𝑖 𝑑𝑖2 𝑖
= =
dSA Surface Area σ 𝑛𝑖 σ 𝑓𝑖൘ 3
𝑑𝑖

1
3 σ 𝑛𝑖 𝑑𝑖3 = 3
dV Volume =
σ 𝑛𝑖 σ 𝑓𝑖൘ 3
𝑑𝑖
Example 1

For this sieve analysis, determine: Mass


Size (µm)
(gram)
800 - 700 0
a) The Sauter mean diameter 700 - 600 5
b) The equivalent volume diameter 600 - 500 50
500 - 400 100
c) The mass mean diameter 400 - 300 50
d) The d50 diameter 300 - 200 15
200 - 0 0
Avg size Mass
Size (mm)
(mm) (gram) Fraction Cum Frac < fi/di fi/di^3 fidi
800 - 700 750 0 0 1.0000 0 0 0
700 - 600 650 5 0.023 1.0000 3.5E-05 8.28E-11 14.773
600 - 500 550 50 0.227 0.9773 0.000413 1.37E-09 125.000
500 - 400 450 100 0.455 0.7500 0.00101 4.99E-09 204.546
400 - 300 350 50 0.227 0.2955 0.000649 5.3E-09 79.546
300 - 200 250 15 0.068 0.0682 0.000273 4.36E-09 17.045
200 - 100 150 0 0 0.0000 0 0 0
Total 220 1 0.00238 1.61E-08 440.909

1 1
𝑑𝑆 = = = 420,1 𝜇𝑚
𝑓𝑖
σ ൗ𝑑 0.00238
𝑖

dSA = 384.5 µm
Mass mean (Average) dm = (fidi)

dV = 396.0 µm
1.00

Size (mm)
Avg size (m) Cum Frac < 0.75
800 - 700 750 1.0000
700 - 600 650 1.0000
0.50
600 - 500 550 0.9773
500 - 400 450 0.7500
400 - 300 350 0.2955 0.25
300 - 200 250 0.0682
200 - 100 150 0.0000
0.00
Total 200 300 400 500 600 700 800

d50 = 445 µm
Bulk properties

Porosity (Ɛ)

𝑂𝑝𝑒𝑛 𝑣𝑜𝑙𝑢𝑚𝑒 (𝑉𝑜𝑝𝑒𝑛 ) 𝑉𝑠𝑜𝑙𝑖𝑑𝑠


𝜖= =1−
𝑇𝑜𝑡𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒 (𝑉𝑇 ) 𝑉𝑇

𝑀𝑎𝑠𝑠 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒𝑠
𝜌𝐵 =
𝑇𝑜𝑡𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒
𝜌𝐵
𝑀𝑎𝑠𝑠 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒𝑠 𝜖 = 1−
𝜌𝑠 = 𝜌𝑠
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒𝑠
Surface area

𝑆𝑢𝑟𝑓𝑎𝑐𝑒 𝑎𝑟𝑒𝑎 𝑜𝑓 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒 6 𝑚2ൗ


𝑆𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑠𝑢𝑟𝑓𝑎𝑐𝑒 𝑎𝑟𝑒𝑎 (𝑆) = =
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒 𝑑𝑆 𝑚3 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒𝑠

6 𝑚2ൗ
𝑃𝑎𝑟𝑡𝑖𝑐𝑙𝑒 𝑎𝑟𝑒𝑎 𝑝𝑒𝑟 𝑢𝑛𝑖𝑡 𝑚𝑎𝑠𝑠 𝑆𝑊 = 𝑘𝑔 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒𝑠
𝜌𝑆 𝑑𝑆

𝑃𝑎𝑟𝑡𝑖𝑐𝑙𝑒 𝑎𝑟𝑒𝑎 𝑝𝑒𝑟 𝑢𝑛𝑖𝑡 𝑏𝑒𝑑 𝑣𝑜𝑙𝑢𝑚𝑒 𝑆𝐵 =𝑆 1−𝜖 𝑚2ൗ


𝑚3 𝑏𝑒𝑑
Gaudin-Schuhmann distribution
𝑛 F(d) = cumulative fraction passing
𝑑
𝐹(𝑑) = d = particle diameter
𝑑𝑒 de and n = constants

Rosin-Rammler (Weibull) distribution

𝑛 F(d) = cumulative fraction passing


− 𝑑ൗ𝑑 d = particle diameter
𝐹 𝑑 = 1−𝑒 𝑒
de and n = constants

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