BS 5 Centrifugation

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    Comparison between filtration and centrifugation:

    Feature Filtration Centrifugation

    Separation principal

    Employment

    Product obtained

    Expense of equipment

    Particle size

    Removal of

    insolubles

    which are

    dilute, large

    and rigid

    Dry cake

    Less

    Density

    Used when

    filtration is

    ineffective

    A pasteor a more

    concentrated

    suspension

    More

    I ntroduction (2/8)

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    Separation costfor recovering whole cells or cell debris:I ntroduction (3/8)

    Ultrafiltration

    more

    economical

    Centrifugation

    more

    economical

    Ultrafiltration

    Centrifugation

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    Schematic presentation ofa laboratory centrifuge:I ntroduction (4/8)

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    Care of centrifuges:(1) Avoid imbalancein the rotor, which may be caused by:

    a. Tube crackingduring the run

    * Conventional glass (Pyrex) centrifuge tubes

    withstand only 34000 g.Use centrifuge tubes made from

    polypropylene or polycarbonate.

    b. Misbalanceof the tubesin the first place

    Small tubesbalanced by volume by eye; large

    tubes (> 200 mL)should be weighed.

    (2) Any spillage should be immediatelyrinsed away.

    Avoid corrosion of centrifuge rotors.

    (3) Do notuse the machine at top speed constantly.

    I ntroduction (5/8)

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    ________________________________________________________________________

    I ntroduction (6/8)

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    * Relative Centrifugal Force, RCF=g

    r2

    1s1047.0

    s60

    min

    min

    2rpm1

    -

    g= 980 cm/s2

    r: in cm

    )((rpm)10119.1

    cm/s980

    cm)(rpm

    s1047.0rpm)(

    RCF 252

    21

    2

    r

    r-

    -

    Often an average RCF is determined using a value for rmidway between the top and bottom of the sample

    container.

    I ntroduction (7/8)

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    ravg= 7 cm

    20,000 rpm RCF = 31,000(centrifugal force = 31,000 g)

    I ntroduction (8/8)

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    FORCES DEVELOPED IN CENTRIFUGAL

    SEPARATION

    The acceleration from a centrifugal force: a= 2rwhere = angular velocity, rad/s

    r= radial distance from center of rotation

    Settling by gravity force: gd

    v sg )(18

    2

    -

    Settling in centrifuges: r

    d

    v s2

    2

    )(18 -

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    Gravitational sedimentation istoo slow to be practicalfor bacteria, and conventional centrifugation is too slow

    for protein macromolecules.

    FORCES DEVELOPED IN CENTRIFUGAL SEPARATION (2/3)

    __________

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    [Example] A laboratory bottle centrifuge is used to collect

    yeast cells after fermentation. The centrifuge consists of a

    number of cylinders rotated perpendicularly to the axis of

    rotation. During centrifugation, the distance between the

    surface of liquid and the axis of rotation is 3 cm, and the

    distance from the bottom of the cylinder to that axis is 10 cm.

    The yeast cells can be assumed to be spherical, with a

    diameter of 8.0 mand a density of 1.05 g/cm3. The fluid hasphysical properties close to those of water. The centrifuge is

    to be operated at 500 rpm. How long does it take to have a

    complete separation?

    Solution:

    rd

    dt

    drv s

    22

    )(18

    - td

    r

    rs

    22

    1

    2 )(18

    ln

    -or

    (To be conti nued)

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    Example: laboratory bottle centr ifuge

    Solution (contd):

    td

    r

    rs

    22

    1

    2 )(18

    ln

    -

    t= 0, r= 3 cm; t= ?, r= 10 cm

    Data: d= 8.0 m = 8.0

    10-4

    cm; = 1 cP = 0.01 g/cm-s; s= 1.05 g/cm3; = 1.0 g/cm3;rad/s3.52

    60

    2500rpm500

    t-

    -2

    24

    )3.52()105.1(01.018

    )100.8(

    3

    10ln

    t= 2467 s = 41.3 min#

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    * Sedimentation Coefficient, s

    The velocity of a particle through a viscous medium

    is usuallyproportional to the accelerating field.

    rd

    v s2

    2

    )(18

    - )(18

    2

    - sd

    s

    Unit of s:svedberg(S; 1 S = 10

    13second)

    Svedberg: the inventorof ultracentrifuge

    rsv 2

    FORCES DEVELOPED IN CENTRI FUGAL SEPARATION (3/3)

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    [Example] Estimate the time it would take to completely

    clarify a suspension of 70 Sribosomes in a high speed

    centrifuge operating at 10,000 rpm. During centrifugation,

    the distance between the surface of liquid and the axis of

    rotation is 4 cm, and the distance of travel of particles

    radially outward is 1 cm.

    Solution:

    5

    4

    2

    0

    1

    r

    dr

    sdt

    t

    h8.1s29080

    s60

    min1

    rev

    2

    min

    rev10000s1070

    223.045ln1 2

    13

    2

    - st

    #

    rsdt

    drv 2

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    TUBULAR BOWL CENTRIFUGE (3/6)

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    The movement of the particle in the z

    direction(due to the convection of the

    feed flow):

    )( 212

    0 RR

    Q

    dt

    dz

    -

    where Q= the volumetric flow rateR1= the distance of liquid interface

    from the axis of rotation

    The movement of the particle in the rdirection:

    rd

    dt

    drs

    22

    )(18

    -

    gd

    v sg )(

    18

    2

    -

    g

    rv

    dt

    drg

    2

    TUBULAR BOWL CENTRIFUGE (3/6)

    TUBULAR BOWL CENTRIFUGE (4/6)

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    )( 212

    0 RR

    Q

    dt

    dz

    -

    g

    rvdt

    drg

    2

    ;

    The trajectory of a particle in the

    centrifuge:

    Q

    RR

    g

    rv

    dtdz

    dtdr

    dz

    drg

    )(

    /

    /2

    1

    2

    02 -

    Consider a particle enters the centrifuge at R1(that is,

    at z= 0, r= R1)anddo not reach R0until at z =

    Q

    RR

    g

    v

    R

    R g )(ln

    2

    1

    2

    0

    2

    1

    0 -

    )/ln(

    )(

    10

    22

    1

    2

    0

    RRg

    vRRQ

    g -

    or

    TUBULAR BOWL CENTRIFUGE (4/6)

    TUBULAR BOWL CENTRIFUGE (5/6)

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    For R0and R1being approximately equal,

    )/ln(

    )(

    10

    22

    1

    2

    0

    RRg

    vRRQ

    g -

    2101

    110

    1010

    110

    1010

    10

    2

    1

    2

    0 2)(/)(

    ))((

    ]/)(1ln[

    ))((

    )/ln(RRRR

    RRR

    RRRR

    RRR

    RRRR

    RR

    RR

    -

    --

    -

    -

    -- 4324

    1

    3

    1

    2

    1)1ln( xxxxxNote:

    )(222

    gg v

    gRvQ

    Note: vgis a function only of the particles themselves,and is a function only of the particular centrifuge.

    TUBULAR BOWL CENTRIFUGE (5/6)

    TUBULAR BOWL CENTRIFUGE (6/6)

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    * Continuous tubular bowl

    centrifugefor separation of

    two liquids:

    An internal baffleprovides a

    separate passage adjacent to

    the bowl wall to conduct the

    heavier-phase liquid to a

    different discharge elevation.

    TUBULAR BOWL CENTRIFUGE (6/6)

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    [Example] A bowl centrifuge is used to concentrate a

    suspension of Escher ichia coli prior to cell disruption. The

    bowl of this unit has an inside radius of 12.7 cmand alength of 73.0 cm. The speed of the bowl is 16,000 rpmand

    the volumetric capacity is 200 L/h. Under these conditions,

    this centrifuge works well. (a) Calculate the settling

    velocity vgfor the cells. (b) After disruption, the diameter of

    debris is about one-half of that of cell and the viscosity is

    increased four times. Estimate the volumetric capacity of

    this same centrifuge operating under these new conditions.

    Solution:

    22

    22

    2or

    2

    R

    Qgv

    g

    RvQ gg

    (To be conti nued)

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    [Example] Analysis of bowl centrifuge

    222

    R

    Qgvg

    Solution:

    Data: R =12.7 cm; = 73 cm; = 16,000 rpm = 1674.7 rad/s;Q= 200 L/h = 55.56 cm3/s; g= 980 cm/s2

    vg= 2.63 10-7cm/s

    Using the same centrifuge,1

    2

    1

    2

    1

    2

    g

    g

    g

    g

    vv

    vv

    QQ

    gd

    v sg )(18

    2

    -16

    1

    4

    )2/1(

    /

    /

    /

    / 2

    12

    2

    1

    2

    2

    1

    2

    1

    2

    2

    2

    1

    2

    dd

    d

    d

    Q

    Q

    (a) Calculate the settling velocity vgfor the cells.

    (b) Estimate the volumetric capacity of this same centrifuge for celldebris.

    #

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    [Example] Beer with a specific gravity of 1.042and a

    viscosity of 1.4 10-3N-s/m2contains 1.5% solids, whichhave a density of 1160 kg/m3. It is clarified at a rate of 240

    L/hin a bowl centrifuge, which has an operating volume of0.09 m3and a speed of 10,000 rev/min. The bowl has a

    radius of 5.5 cmand is fitted with a 4-cm outlet. Calculate

    the effect on feed rate of an increase in bowl speed to 15,000

    rev/min andthe minimum particle size that can be removed

    at the higher speed.

    Solution:

    All conditions except the bowl speedremain the same.

    2

    1

    2

    2

    1

    2

    Q

    Q

    )]([)]/[ln(18

    )(

    )/ln(

    )(2

    1

    2

    010

    22

    10

    22

    1

    2

    0RR

    RR

    d

    RRg

    vRRQ s

    g --

    -

    (To be conti nued)

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    Calculate: when = 15,000 rev/min, Q= ? d= ?Solution (contd):

    )]([)]/[ln(18

    )( 21

    2

    0

    10

    22

    RRRR

    dQ s -

    -

    2

    1

    2

    2

    1

    2

    Q

    Q 2

    22

    )10000(

    )15000(

    240

    Q

    /sm105.1s3600

    h

    L1000

    mL/h540 34

    3

    2

    -

    Q

    [Example] Beer with a specific gravity of 1.042and a viscosity of 1.4 10-3N-s/m2contains 1.5% solids, which have a density of 1160 kg/m3. It

    is clarified at a rate of 240 L/hin a bowl centrifuge, which has an

    operating volume of 0.09 m3and a speed of 10,000 rev/min. The bowlhas a radius of 5.5 cmand is fitted with a 4-cm outlet.

    (To be conti nued)

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    )]([

    )]/[ln(18

    )( 21

    2

    0

    10

    22

    RR

    RR

    dQ s -

    -

    1s157060

    215000 -

    Operating volume32

    1

    2

    0 m09.0)]([ - RR

    ]09.0[)4/5.5ln()104.1(18

    )10421160()1570(105.1

    3

    224

    -

    -

    -

    d

    d= 2.14 107m

    Calculate: when = 15,000 rev/min, Q= ? d= ?Solution (contd):

    [Example] Beer with a specific gravity of 1.042and a viscosity of 1.4 10-3N-s/m2contains 1.5% solids, which have a density of 1160 kg/m3. It

    is clarified at a rate of 240 L/hin a bowl centrifuge, which has an

    operating volume of 0.09 m3and a speed of 10,000 rev/min. The bowl

    has a radius of 5.5 cmand is fitted with a 4-cm outlet.

    #

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    SEPARATION OF L IQUIDS BY CENTRI FUGATION (2/3)

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    The differential force across a

    thickness dris:dF= r2dm

    r

    dFdPrdrdm

    2and])2[(

    rdrr

    rdrrdP

    22

    2

    ])2[(

    -

    Integration between r1and r2:

    21222

    212

    rrPP --

    SEPARATION OF L IQUIDS BY CENTRI FUGATION (2/3)

    SEPARATION OF L IQUIDS BY CENTRI FUGATION (3/3)

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    21222

    212

    rrPP --

    At the liquid-liquid interface,

    Pressure exerted by the light

    phase of thickness (r2 r1)

    = Pressure exerted by the heavyphase of thickness (r2 r4)

    21222

    2

    4

    2

    2

    2

    22rrrr LH --

    LH

    LH rrr

    -

    -

    21

    242

    2

    * The interface at r2must be located at a radius smaller

    than r3.

    SEPARATION OF L IQUIDS BY CENTRI FUGATION (3/3)

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    [Example] In a vegetable-oil-refining process, an aqueous

    phase is being separated from the oil phase in a centrifuge.

    The density of the oil is 919.5 kg/m3and that of the aqueous

    phase is 980.3 kg/m3. The radius for overflow of the light

    liquid has been set at 10.160 mmand the outlet for the

    heavy liquid at 10.414 mm. Calculate the location of the

    interface in the centrifuge.

    Solution:

    LH

    LH rrr

    -

    -

    2

    1

    2

    42

    2

    5.9193.980

    )160.10(5.919)414.10(3.980 2222

    -

    -

    r

    r2= 13.75 mm#

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    DISK CENTRIFUGE

    DI SK CENTRIFUGE (2/14)

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    A short, wide bowl8 to 20 in.in diameter turns on a verticalaxis. Inside the bowl and

    rotating with it are closely

    spaced disks,which are

    actually cones of sheet metal

    set one above the other.

    In operation, feed liquidenters the bowl at the bottom,

    flows into the channels, and

    upward past the disks.

    DI SK CENTRIFUGE (2/14)

    DI SK CENTRIFUGE (3/14)

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    The operation can be made continuous.DI SK CENTRIFUGE (3/14)

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    ___

    ____

    ___

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    Collection of solid:

    DI SK CENTRIFUGE (6/14)

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    A properly operated disc centrifuge should separate99% of the solids from the liquid streamand produce

    an 8090% wet solids concentrate. The smaller the particle diameter, the lower the flow

    rate, and the longer the interval between discharges.

    * Flow rate is proportional to the square of thediameter of the particle.

    gd

    vvQ sgg )(18

    ;2

    -

    * Cell debris (particle size 0.5 m)can beseparated with flow rates of 300500 L/h.

    ( )

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    DI SK CENTRIFUGE (8/14)

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    Consider a particle located

    at position (x, y), where xis

    the distance from the edge

    of the outer disks along the

    gapbetween the disk, and

    yis the distance normal to

    the lower disk. Liquid isfed into the centrifuge so

    that it flows upward

    through the gap between

    the disks, entering at R0and leaving at R1.

    ( )

    DI SK CENTRIFUGE (9/14)

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    The velocity of the particle in the xdirection is:

    sin0 vvdtdx -

    where v0is the convective liquid velocity, and vis theparticles velocity under centrifugation.

    ( )

    DISK CENTRIFUGE (10/14)

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    There are three important characteristics of v0:

    (1) Under most conditions, v0>> vsin.(2) v0is a function of radius.

    (3) v0is a function of y.

    )()2(

    0 yfrn

    Qv

    dt

    dx

    where Q= the total volumetric flow rate

    n= number of disks

    r= the distance from the axis of rotation

    = the distance between disks

    f(y) = some function giving the velocity variation

    across the distance between disks

    DI SK CENTRIFUGE (11/14)

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    )()2(

    0 yfrn

    Qv

    dt

    dx

    Note: Q= (total cross sectional area)(average velocity)

    dy

    rn

    yQfrndyvrnQ

    00

    0

    )2(

    )(1)2(

    1)2(

    1)(1

    0

    dyyf

    DISK CENTRIFUGE (12/14)

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    The velocity of the particle in the ydirection is:

    coscos2

    g

    rvv

    dt

    dyg

    The trajectory of a particlebetween the disks of this

    centrifuge is:

    cos)(

    2

    /

    / 22

    ryQgf

    vn

    dtdx

    dtdy

    dx

    dy g

    )()2(

    0 yfrn

    Qvdtdx

    DISK CENTRIFUGE (13/14)

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    cos)(

    2

    /

    / 22

    ryQgf

    vn

    dtdx

    dtdy

    dx

    dy g

    sin0 xRr -

    cos)sin()(

    2 20

    2

    xRyQgf

    vndxdy g -

    sin0 xRr -

    DISK CENTRIFUGE (14/14)

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    sin0 xRr -

    cos)sin()(

    220

    2

    xRyQgf

    vn

    dx

    dy g-

    Integration for those particlesthat are most difficult to

    capture,that is,

    At x= 0, y= 0 (The most unfavorable entering position.)

    At x= (R0 R1)/sin, y= (They are captured at the wall.)

    )(cot)(3

    2 31

    3

    0

    2

    - gg vRR

    g

    nvQ

    1)(1

    0

    dyyf

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    [Example] Chlorella cells are being cultivated in an open

    pond. We plan to harvest this biomass by passing the dilute

    stream of cells through an available disc bowl centrifuge.

    The settling velocity vgfor these cells has been measured as1.07 10-4cm/s. The centrifuge has 80 discswith an angle of40, an outer radius of 15.7 cm, and an inner radius of 6 cm.We plan to operate the centrifuge at 6000 rpm. Estimate the

    volumetric capacityQ

    for this centrifuge.

    Solution:

    -

    cot)(

    3

    2 31

    3

    0

    2

    RRg

    nvQ g

    Data: vg= 1.07 10-4cm/s; n= 80; R0= 15.7 cm; R1= 6 cm; = 40; g=980 cm/s2

    rad/s62860

    26000

    Q= 3.14 104cm3/s = 31.4 L/s

    #

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    SCALEUP OF CENTRIFUGATION

    Use laboratory data to predict performance of

    commercially available centrifuges.

    Commercially available centrifuges are designed on amechanical basisand cannot be modified easily.

    Laboratory bottle centrifuges, being batch operation,give a clear liquid and a concentrated solid or paste.

    An idealized separation, never reached in a

    continuous flow centrifuge.

    There are two approaches of scaleup of centrifugation:(1) use of the equivalent time Gt

    (2) sigma analysis

    SCALEUP OF CENTRIFUGATION (2/5)

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    Scaleup of centrifugation based on the equivalent time GtGt: a measurement of the difficulty of a given separation

    tg

    RGt

    2

    where R= a characteristic radius, often the maximum

    in the centrifuge

    t= the time needed for a particle to reach R

    * Once the value for Gtis determined, a large-scale

    centrifuge that has a similar Gtshould be considered.

    * This approach must be regarded as only a crude

    approximation.

    SCALEUP OF CENTRIFUGATION (3/5)

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    Values of Gtfor various solids:

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    [Example] It has been shown that bacterial cell debris

    has Gt= 54 106s. For a centrifuge bowl of 10 cmindiameter, find the centrifuge speedif a fullsedimentation in 2 his required.

    Solution:

    tg

    RGt

    2

    )36002(980

    )5(

    1054

    26

    rpm580,11min

    s60

    rad2

    rev1rad/s1212

    #

    SCALEUP OF CENTRIFUGATION (4/5)

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    Scaleup of centrifugation using the factor (Q= vg)Scaleup involves choosing a centrifuge that hasthe required valueto meet the processrequirements of vgand Q.

    * The value of is really the area of a gravitationalsettlerthat will have the same sedimentation

    characteristics as the centrifuge for the same feed

    rate.

    SCALEUP OF CENTRIFUGATION (5/5)

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    Scaleup of centrifugation using the factor (Q= vg)

    * Scaleup from a laboratory test of Q1and 1to Q2using similar type and geometry centrifuges:

    2

    2

    1

    1

    QQ

    * Scaleup if different centrifuges are used:

    22

    2

    11

    1

    E

    Q

    E

    Q

    Eis the efficiency of a centrifuge, which is determined

    experimentally.

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    [Example] Recovery of starch particles.

    = 10-3kg/m-s; s= 100 kg/m3(a) Calculate the effective diameter of the starch particles.

    Solution:

    m/s1066.5s60

    min

    ft3.28

    m

    gal7.48

    ft

    ft1202

    gal/min2 63

    2

    -

    gv

    A starch table with the dimensions of 2 ft wide and120 ft longcan

    handle a slurry feed rate of 2 gal/min.

    gdv sg )(18

    2

    - )8.9)(100()10(18

    1066.53

    26

    --

    d

    d= 1.02 10-5m(To be continued)

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    [Example] Recovery of starch particles. The centrifuge has a value of31,500 m2. (b) Estimate the centrifuge throughput, assuming that you

    can operate at 50% of the theoretical maximum.

    Solution (contd):

    Qat 50% of the theoretical maximum

    = vg(0.5) = (5.66 10-6) (0.5 31500)

    gal/min1410min

    s60

    L28.32

    gal7.48

    m

    L1000

    s

    m089.0

    3

    3

    #

    m/s1066.5 6-gv

    [Example] A new recombinant protein is produced in

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    [Example] A new recombinant protein is produced in

    yeast. The company scientists, also known as the boys in

    the lab,separate the cells in a laboratory bottle centrifuge

    to give a thick paste that will be subsequently disrupted to

    release the protein. This separation is accomplished by

    centrifuging small quantities of the broth for 30 minat

    2000 rpm. In the lab centrifuge, the inner radius of the

    solution is 5 cmand the bottle tip radius is 15 cm. The cell

    suspension contains only 7% by volume of cells. We areasked to recommend the size and type of centrifuge for

    separating 10 m3 of this suspension per day.

    Solution:

    g

    rv

    dt

    drg

    2 t

    gR

    R

    dtg

    v

    r

    dr

    0

    20

    1

    t

    RRgv

    g

    tv

    R

    Rg

    g

    2

    10

    2

    1

    0 )/ln(orln

    (To be continued)

    Q= vg

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    [Example] Recommend the size and type of centrifuge for separating

    10 m3 of a yeast suspension per day.

    t

    RRgvg 2

    10 )/ln(

    Solution (contd):

    Data: R1= 5 cm; R0= 15 cm; t= 30 min; = 2000 rpmvg= 1.36 105cm/s

    2

    5

    3

    m851

    cm/s101.36

    day/m10

    -

    gv

    Q

    * In general, a safety factor of 2is introduced for disc

    centrifuges, while no safety factor is neededfor tubular

    bowl centrifuges.

    #

    [Example] We want to centrifuge chlorella cells using an

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    [Example] We want to centrifuge chlorella cells using an

    available disc bowl centrifuge operated at 6000 rpm. The

    centrifuge has 80 discswith an angle of 40, an outer radiusof 15.7 cm, and an inner radius of 6 cm. The cell suspensionhas a viscosity of 1 cpand a density difference of 0.1 g/cm3.

    The effective diameter of chlorella cells is 4.3 104cm.Assume the efficiency of the disc centrifuge is 0.5; estimate

    the throughput.

    Solution:

    cm/s1001.1)980)(1.0()01.0(18

    )103.4()(

    18

    4242

    --

    - gd

    v sg

    1s628s60

    min

    rev

    2rev/min6000 -

    - ERR

    g

    nvQ g

    cot)(

    3

    2 31

    3

    0

    2

    = 14,820 cm3/s

    #

    s-cm

    g:poise

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    SCROLL TYPE OF DECANTING CENTRIFUGE

    Horizontal Type

    * An internal scroll conveyoris used to move the decanted

    solid out of the machine.

    * Centrifugal force: 5006,000 g

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    * Scroll Decanting

    Centrifuge: Vertical

    Type (2/2)

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    ULTRACENTRIFUGE

    The term ultracentrifuge was originally applied by T.Svedbergto any centrifuge that permitted observation of

    the contents of the container during the act of

    centrifuging.

    It is now more commonly applied to any ultrahigh-forcecentrifuge(up to 75,000 rpm, with RCF values up to

    500,000 g).

    ULTRACENTRIFUGE (2/3)

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    ULTRACENTRIFUGE (3/3)

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    SELECTION OF EQUIPMENT FOR LIQUID-

    SOLID SEPARATIONS

    Major function:

    (1) Recover solids

    (2) Clarify liquid

    Operation mode:

    (1) Continuous

    (2) Batch, automatic(3) Batch

    Major function Operation Classification

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    Classification Equipment Subclassification

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    Major function Operation Classification

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    Classification Equipment Subclassification

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    CENTRIFUGAL EXTRACTOR

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    CENTRIFUGAL EXTRACTOR

    CENTRIFUGAL EXTRACTOR (2/2)

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