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    Chapter 1

    Characterization Of Individual Particles

    Cedric Briens April 16, 2010

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    1. Introduction

    1.The design of any operation involvingparticles requires precise information on

    their properties2.The most important properties are density,

    size and shape

    3.This chapter defines these properties andreviews the techniques for theirmeasurement

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    Outline

    1 Introduction

    2 Particle density

    3 Particle size

    4 Particle shape

    5 Adhesion of particles6 Dustiness

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    2. Particle density

    Skeletal density

    Apparent particle density

    Bulk density

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    What is the Skeletal density?

    Density of the material from which particles

    are formed: rsk

    non-porouss

    non-porouss

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    What is the

    apparent particle density?

    non-porouss

    p

    mass of particle

    volume of particle (including pores)r

    non-porouss

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    Relationship between rpand rsk

    p

    p sk

    1 1

    r rvolume of solid material volume of pores

    solid mass

    volume of solid material volume of pores

    solid mass solid mass

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    What is the bulk density?

    Density of the bulk

    powder: includes the voids in-

    between the particles

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    Relationship between rb= rp

    b p 1r r

    : voidage or volume fraction of bulk powder

    occupied byvoids.

    mass of solid mass of solid volume of bed volume of voids

    volume of bed volume of particles volume of bed

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    Example:

    fluidized cracking catalyst

    rsk= 2500 kg/m3

    p= 0.50x10-3m3/kg

    rp= 1100 kg/m3

    rb= 500 kg/m

    3

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    Bulk density measurement

    The bulk density depends on how the powder

    is packed

    Two extremes:

    Loose or aerated bulk density

    Compact or tapped bulk density

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    Bulk density measurement

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    Loose or aerated bulk density

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    Compact or tapped bulk density

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    Skeletal density measurement

    Two pycnometry measurement techniques

    may be used:

    1) liquid pycnometry: inaccurate

    2) gas pycnometry: elaborate but accurate

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    Liquid pycnometry

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    Liquid pycnometry

    weighing mass of added water volume of added water

    volume of flask volume of added water volume of solids material

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    Liquid pycnometry

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    Liquid pycnometry

    Porous particles:

    The liquid may

    not fill allthe

    pores

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    Gas pycnometry

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    Particle density measurement

    1) Mercury pycnometry: assume that

    mercury does not penetrate into the pores(Mercury is sometimes replaced bysilicone oil).Inaccurate

    2) Caking detection: caking occurs whenthe pores are filled with liquid.Inaccurate

    3) Gas adsorption isotherms

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    Outline

    1 Introduction

    2 Particle density

    3 Particle size

    4 Particle shape

    5 Adhesion of particles

    6 Dustiness

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    FCC

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    FCC

    tertiarycyclone

    catch

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    Talcumpowder

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    Polymer C

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    Polymer W

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    Polymer E

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    Characterizing the size of a

    particle with a complex shape

    Volume-equivalent particle diameter: diameter of

    the sphere which has the same volume as the particle

    Others:

    Aerodynamic diameter: diameter of the sphere with a density of

    1000 kg/m3

    which falls at the same speed as the particle in ambientair

    Sieve diameter

    Diameters based on projected area

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    Particle size cuts

    Size cut i contains

    the particles with a

    diameter between

    dpi- Ddpi/2

    and

    dpi+ Ddpi/2

    particle diameter (dp), m

    0 50 100 150 200 250 300 350 400 450 500 550 600

    fraction

    ofparticles

    in

    size

    cut(x i)

    0.00

    0.02

    0.04

    0.06

    0.08

    0.10

    0.12

    0.14

    0.16

    0.18

    ximay be based on:weight

    volume

    area

    number

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    Mean diameters

    pam i pi i

    i i

    plm i pi

    i

    i

    i

    i

    psm pi

    : d x d (note : x 1)

    : ln d x ln d

    For the arithmetic and log mean diameters, x may be any type of fracti

    arithmetic mean

    geometric or log mean

    Sauter me

    on

    For the , x be the volume fracmu tist on :

    1 x

    an

    d d

    diameter

    i

    S di d

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    Sauter-mean diameter and

    specific area

    p psm

    p psm

    mean specific surface (a):

    particle surface in 1 kg of mixed size solids

    6spherical particles: a

    d

    6non-spherical particles: a

    d

    r

    r

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    Median particle diameter

    Diameter such that 50% of particles are

    larger than this diameter and 50% aresmaller

    The median diameter depends on the type of

    fraction xi

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    Comparison of various mean diameters for a typical size distribution

    arithmetic mean diameter, m 221

    from log-mean or geometric mean diameter, m 168

    volume % harmonic or Sauter mean diameter, m 99

    median diameter, m 192

    arithmetic mean diameter, m 1.3

    from log-mean or geometric mean diameter, m 1.0

    number % harmonic mean diameter, m 0.9

    median diameter, m 0.8

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    Cumulative distribution

    particle diameter (dp), m

    0 100 200 300 400 500 600

    weigh

    t%

    withadiametersmallerthandp

    0

    10

    20

    30

    40

    50

    60

    70

    80

    90

    100

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    Differential distribution

    particle diameter (dp), m

    0 100 200 300 400 500 600

    derivative,wt%

    /m

    0.0

    0.1

    0.2

    0.3

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    Relationship between number and

    weight distributions

    Use Excel (or FBMODX)

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    Combining two particle size

    distributions of the same sample

    For example, two measurement techniques

    may provide the size distribution of asample for 2 different ranges of particle size

    The easiest way is to use the cumulative

    distribution

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    Theoretical size distribution

    functions

    Useful for smoothing and interpolation

    Do notuse for extrapolation

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    Normal or gaussian distribution

    p

    2

    pi pam2

    d

    p pi0

    d dexp2

    F(d ) d(d )

    2

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    Log-normal distribution

    F d

    d

    d

    d dd

    p

    pi

    plm

    g

    g

    pi

    pi

    dp( )

    expln

    ln

    ln

    ( )

    2

    2

    0

    2

    2

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    Rosin-Rammler distribution

    s

    pp daexp1)d(F

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    Weibul distribution

    pm

    minpp

    d

    ddX

    Xexp1dF p

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    Normal paper

    If the distribution is gaussian, thecumulative distribution

    will plot as a straight line

    particle diameter (dp), m

    0 100 200 300 400 500 600

    weight%withadiametersmaller

    thandp

    0.001

    0.01

    0.1

    1

    10

    30

    50

    70

    90

    99

    99.9normal probability paper

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    Log-normal paper

    If the distribution is log-normal, thecumulative distribution

    will plot as a straight line.

    particle diameter (dp), m

    1 10 100

    weight%w

    ithadiametersmalle

    rthandp

    0.001

    0.01

    0.1

    1

    10

    30

    50

    70

    90

    99

    99.9log-normal probability paper

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    Particle size measurement

    Accurate sampling is a crucial operation: moreerrors can be attributed to sampling than to theactual size analysis.

    The two "golden rules of sampling" (Allen):

    1) "a powder should be sampled while in motion" (toprevent segregation in non- moving powders)

    2) "the whole of the stream should be taken for manyshort increments of time in preference to part of the

    stream being taken for the whole of the time"(segregation).

    With fine particles, sample dispersion is alsoimportant.

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    Particle size measurement

    i l i

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    Particle size measurement

    i l i

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    Particle size measurement

    Various methods:

    1) Sieving: usually for dp> 50 m

    2) Sedimentation or centrifugation in a liquid

    3) Centrifugation in a gas

    4) Elutriation

    5) Impaction

    6) Electrical conductivity7) Light scattering and blockage

    8) Image analysis

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    Sieving

    Si i

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    Sieving

    Si i

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    Sieving

    time consuming shaking duration must be long enough to prevent

    large errors

    cannot be used with solids which attrit oragglomerate easily

    if angular particles, does not give volume-equivalent diameter

    Sieving results are often reported in terms of meshnumbers: a large mesh number means a small

    particle size

    Li h i

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    Light scattering

    The most popular technique

    Measures the projected area of the particles and

    thus provides the volume-equivalent diameterwhen the measurement cell is designed so as to

    present the particles in a random orientation

    Measures particle diameters from 0.5 to 3000 m

    Both dry and wet measurements

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    Dry methods: screening,elutriation,centrifugation in a gas, impaction, light

    scattering

    A frequent problem with these methods:

    Particle-particle agglomeration due to Van der

    Waals or electrostatic forces

    Prevalent for small particles (high surface/volume)

    Additives can help

    h d

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    Wet methods:sedimentation/centrifugation, electrical

    conductivity, light scattering

    Particle-particle agglomerates can be broken apartby a combination of surfactant additives and

    ultrasonic vibrations

    Surfactants may also promote agglomeration

    Ultrasonic vibrations may promote agglomeration

    or break particles

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    Outline

    1 Introduction

    2 Particle density

    3 Particle size

    4 Particle shape

    5 Adhesion of particles

    6 Dustiness

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    4. Particle shape

    Introduction

    Various shape factors

    Shape factors from direct shape characterization

    Shape factors from particle-fluid interactions

    Shape factors from product quality tests

    Measurement of particle shape

    P ti l h l

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    Particle shape: examples

    - inks, paints, cosmetics: flaky particles cover morearea

    - abrasives: better if highly angular

    - fibers for plastics reinforcement: elongated forgood impact strength.

    - rubber grains: must be round for good tensile

    strength (otherwise, grains would align along onedirection and eventually tear)

    - perfectly spherical particles have a smoother feelattractive for cosmetic applications

    Shape factors from direct shape

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    Shape factors from direct shape

    characterization

    Usually from image analysis

    Example: for each particle, draw diameters

    through its center of gravity, 30 degrees apart,and take the ratio of the smallest to the largestof these diameters

    surface area of sphere with the same volume as the particle

    actual surface area of the particle

    Particle sphericity:

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    Shape factors from particle-fluid

    interactions

    Many shape factors based on measured

    particle-fluid interactions

    See the chapter on Particulate-Fluid

    interactions

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    Shape factors from product

    quality tests Flakiness index

    round particles:

    "flaky" particles:

    Angularity index: based on Hausner ratio:

    Angular particles are more cohesive

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    Outline

    1 Introduction

    2 Particle density

    3 Particle size

    4 Particle shape

    5 Adhesion of particles

    6 Dustiness

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    5. Adhesion of particles

    Adhesion of particles on other particles or

    on a flat surface may be very important forsome processes

    There are very few techniques to

    characterize such adhesion (e.g. theturntable)

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    Outline

    1 Introduction

    2 Particle density

    3 Particle size

    4 Particle shape

    5 Adhesion of particles

    6 Dustiness

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    6. Dustiness

    filter

    solidssample

    suction

    dust