Centrifugation

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Centrifugation

Theory of centrifugation
Types of centrifuges
Applications

Centrifugal separations
Sedimentation operation accelerated
by centrifugal force
Pre-requisite for the separation is a
difference in density between the
phases
This applies to both
solidliquid separation
liquidliquid separation

Sedimentation by
Gravity

A particle suspended in a liquid medium of


lesser density tends to sediment downward
due to the force of gravity (Fg)
Two forces oppose the gravitational force
the buoyancy force, Fb
the frictional force, Ff

Fg mg m 980cm.s

Buoyancy force
Fb mM g V p M g

mM = the mass of the fluid


medium displaced
Vp = the volume of the
particle
M = the density of the
displaced fluid

The net gravitational effect, taking into


account the buoyancy force is

Fg net

4 3
4 3
r P M g r P M 980cm.s 2
3
3
M = the density of the medium
(g.cm-3)
P = the particle density (g.cm-3)
r = the particle radius (cm).

Frictional force
The movement of a particle through a
fluid medium is hindered by the viscosity
of the medium, as described for a
spherical particle by Stokes equation

dx
Ff 6 r
dt
= viscosity of the medium in poise, P (g cm1 -1
s );
r = the radius of the particle (cm);
(dx/dt) = the velocity of the moving particle
(cm.s-1).

Frictional force
At low velocities and pressures, the frictional
force is negligible in a gas.
At higher velocities, even in gases, this force
becomes substantial, combining with the
buoyancy force eventually to exactly oppose
the gravitational force, resulting in no further
acceleration of the particle (the limiting or
terminal
velocity)
Mathematically,
the
conditions for attaining
Fg Fb Ff
terminal velocity are met
when:

Effect of Diffusion
Ficks law:
Random Brownian
motion results in the net
dP
dP
DA
movement of solute or

dt
dx

suspended particles
D = the diffusion coefficient
which varies for each solute
from regions of higher
concentration to regions and particle
of lower concentration
A = the cross sectional area
through which the particle
Diffusion works in
diffuses
opposition to centrifugal
dP/dx = the particle
sedimentation, which
concentration gradient
tends to concentrate
particles

Sedimentation in a
Centrifugal Field

A particle moving in a circular path continuously


experiences a centrifugal force, Fc.
This force acts in the plane described by the circular
path and is directed away from the axis of rotation.
The centrifugal force may be expressed as

Fc ma m x
2

m = the particle mass (g);


a = the acceleration (cm.s-2)
= the angular velocity (radians s-1 .rpm/60)
x = the radial distance from the axis of rotation to the
particle (cm)

Relative centrifugal force (RCF)


Ratio of acceleration of the centrifugal field to that of
acceleration owing to the earths gravity

Fc
RCF

Fg

2
m

mg

Alternatively RCF is given by

RCF 1.119 10

rpm

m = the particle mass (g);


a = the acceleration (cm.s-2);
= the angular velocity (radians s-1 2.rpm/60);
x = the radial distance from the axis of rotation to the
particle (cm).

Forces acting on a particle in a


centrifugal field
When centrifugal force is equaled by
buoyancy and frictional forces

Fc Fb Ff

dx
m x VP M x 6 r
dt
2

Assuming spherical particles the


above equation becomes

Fb = buoyancy
force
Ff = frictional
force
Fc = centrifugal
force

4 3
4 3
dx
2
2
r P x r M x 6 r
3
3
dt
Solving for (dx/dt)

dx

dt

2r 2 P M 2 x
9

Forces acting on a particle in a


centrifugal field
In terms of particle diameter, d and particle
velocity, v
d 2 P M 2 x
v

18

Upon integration the equation above yields the


time required for a particle to traverse a radial
distance from x0 to x1

x1
18
ln
t
2
2
d P M
x0

x0 is the initial position of the


particle
x1 is the final position of the

Parameters that govern


settling velocity
The sedimentation rate of a particle
in a centrifugal field
increases as the square of the particle
diameter and rotor speed
doubling the speed or particle diameter will
lessen the run time by a factor of four

increases proportionally with distance


from the axis or rotation
inversely related to the viscosity of the
carrier medium

Sedimentation Coefficient (Sr)


In a homogeneous medium,
the following parameters
are constant for a given
For a given set of run
particle
conditions

The viscosity
Particle size
Particle density
Density of the medium

The sedimentation rate is


proportional to 2x

dx
2r 2
dt
P
M

Sr 2
9
x

expressed in terms of the


sedimentation coefficient, S.

Measure of the
sedimentation velocity per
unit of centrifugal force

Sedimentation Coefficient
The sedimentation coefficient
has the dimensions of seconds
expressed in Svedberg units equal
to 10-13 s

Sedimentation coefficient is
dependent on

the particle being separated20, w


the centrifugal force
the properties of the
sedimentation medium.

Useful to compare
sedimentation coefficients
obtained
under differing conditions
sedimentation media by reference

ST , MT ,M P M

20,W P T , M

Rotor Efficiency or Pelleting


Efficiency (k-factor)

Pelleting efficiency or k-factor

The time required for a particle to traverse a rotor

k-factor
calculated at the maximum rated rotor speed, is a
function of rotor design and is a constant for a given
rotor.

k-factors are useful for


determining the minimum residence time required to
pellet a particle in a given rotor
comparing sedimentation times for different rotors

he k-factor is derived from the equation

ln rmax rmin 1013


k
3600 2

rmax and rmin are the maximum


and minimum distances from
the centrifugal axis

k 2.53 10 ln rmax rmin / rpm


11

If the sedimentation coefficient of a particle is


known, then the rotor k-factor can also be
calculated from the relation:
T = time in hours required for

k TS

pelleting
S = the sedimentation coefficient
in Svedberg units

For runs conducted at less


than the maximum rated rotor
speed, the k-factor may be
adjusted according to

kadj

rpmmax
k

rpmact

k-Factors are also useful when switching from a


rotor with a known pelleting time, t1, to a second
rotor of differing geometry by solving for t2 in the
relation

em: Separating cells growing on a suppo


Animal cells can be cultivated on the external surface
of dextran beads. These cell laden beads or
microcarriers have a density of 1.02 g/ml and a
diameter of 150 m.
A 50 litre stirred tank is used to cultivate cells grown
on microcarriers to produce a viral vaccine. After
growth, the stirring is stopped and are allowed to
settle. The microcarrier-free fluid is then withdrawn to
isolate the vaccine.
The tank has a liquid height to diameter ratio of
1:1.5; the carrier-free fluid has density of 1 g/ml and
a viscosity of 1.1 cP.
a) Estimate the settling time to reach the velocity

(a)

Using the equation for terminal velocity

Substituting the values we get

2
2
d

P M x

18

v 0.022cm.s 1

du
Re
1
okes law is applicable if the condition is satisfied that

du (0.015cm)(0.022cm / sec)1g / cm3)


Re

0.03

(0.011g / cm.sec)
2
V d l
Hence the use of Stokes equation is justified
4
2

To calculate the liquid height from tank volume


3
3

l

50

10
cm

4 1.5
l 52.3cm

The terminal velocity of the particle can be made


use of to calculate the settling time
t = l/vg = 52.3 cm/0.022 cm/sec = 39.6 min
Approximately it will take 40 min for the
microcarriers to completely settle
(b) Assuming the velocity of the microcarriers is
originally zero we find the change of settling velocity
by a force balance on the particle

d3
dv
Fg Fb FD
P M Fb FD
6
dt
dvg
dt

3 dv

d3
P M
6

18v
g 2
d P M

dvg

3 dv

18v
Subject to initial condition t=0
g 2
d P M and v=0

d3
P M
6
Integrating the above equation we can find that
dt

gd 2 ( p M )
vg

18

1 exp 18 t

2
d
(

p
M

Hence assuming steady state condition where


d 2 ( s p) d 2 ( s p)
t?

18
18
(0.015cm) 2 (0.02 g / cm3 )

2.27 105 sec


18(0.011g / cm.sec)

nce our settling time is 40 minutes we easily meet this criter

oblem: Centrifugation of yeast cells


A laboratory bottle centrifuge consists of a number of
cylinders rotated perpendicular 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 m and a density of 1.05 g/ml.
The fluid has physical properties close to those of pure
water.
The centrifuge is to be operated at 500 rpm.

From the equation


It was found that

d2
v
( s ) 2 r
18
dr
d2
v
( s ) 2 r
r
18

We are interested in the yeast cell which takes longest to settle, which is that
starting near the liquid surface, t = 0; r = 3 cm.
Integrating the initial equation, we find

r
d2
2
ln

18
3cm

Substituting the values, we get

500 2 2
(8 104 cm) 2
g
10cm
ln
0.05


1
1
3
3
cm
18(0.01
g
.
cm
.sec
cm
60sec

t 2500sec

Types of Centrifugal
Separation
According to the phase of the medium and
the phase of the material to be purified
Gas-gas
Liquid-liquid
Liquid-solid

According to the method by which purified


fractions are recovered
Batch mode
Semi-batch mode
continuous mode

Types of centrifuges
Tubular bowl centrifuges
Simple yet can provide very high G
Can be cooled
Disadvantage: Requirement for intermittent
dismantling for cleaning

Disc type centrifuges: Three types


Solids-retaining
Intermittent solids-ejecting
Continuous solids-ejecting

Basket type centrifuges


Used for centrifugal filtration

ubular bowl centrifuge


Utilize a vertically mounted, imperforate
cylindrical-bowl
design to process feed streams with a low
Liquid
is discharged continuously
solids content
and solids are manually recovered
after the rotor capacity is reached
Industrial models are available
with
Diameters up to 1.8 m
Holding capacities up to 12 kg
Throughput rates of 250 m3 h-1
Centifugal forces ranging up to
20000 g.models are available with
Laboratory
Diameters of 4.5 cm
Throughput rates of 150 L.h-1
Centrifugal forces ranging up to
62000g.

Performance analysis of a
tubular centrifuge
Analysis depends on finding the
position of a particle as a
function of time
Assumptions
1. Particle located at a distance z from
the bottom of the centrifuge
2. It is also located at position r from
the axis of rotation
3. This position is between the liquid
surface R1 and bowl radius R0 w
4. Feed freely flows in the bottom and
out the top
5. Solids are thrown out by centrifugal
force and trapped against the wall,
located at R0
6. The centrifugal force is so high that
the liquid interface R is constant

R0

R1

z
r Liquid Interface

Idealization of the tubular


bowl centrifuge

rmance analysis of a tubular centrifuge

article is moving in both the z and r directions.

vement in the z direction comes from the convection of the feed pumped
bottom of the centrifuge

dz
Q

2
2 Q is the feed flow rate
dt ( R0 R1 )

article movement in the r direction is related to its radial position by

dr d 2

s r r 2
dt 18

dr
r

hich can be rewritten in terms the velocity of a


vg

rticle settling under the influence of gravity


dt
g

find the trajectory of the particle within the centrifuge


2
2

r 2
dr dr / dt
0
1

vg

dz dz / dt
Q
g

For particles which are most difficult to capture, they enter


the centrifuge at r=R1 and do not reach r=R0 until the end
of the unit at z=l
Integration and rearrangement of the equation for the
particle trajectory gives the maximum flow possible flow
rate in the centrifuge as a function of both particle
properties and centrifuge
2 characteristics
2
2

l R0 R1 vg
g ln R0 / R1

In most tubular centrifuges as R0 and R1 are


approximately equal, we can simplify the above
equation
2
2

R0 R1 R0 R1

( R0 R1 )

ln( R0 / R1 ) ln 1 R0 R1 / R1
R0 R1 R0 R1

R1 ( R0 R1 )
R0 R1 / R1 ....
2R2

2 lR 2 2
Q vg
v g [ ]

he Generalized Formula
The most-used quantity to characterize centrifuges,
the concept
2
2

Qtheor vg . Where,

Assumptions

2 lR

Viscous drag is determining


the particle movement. The equation for critical diameter become
1
The flow in disk bowls
2
between the disks is laminar
18. .Q

Se
theor
and symmetrical.

dc
.
2 2
p f V . .r
The liquid rotates at the same

speed as the bowl


1
The particle concentration is
2

low (no hindered settling).


18. .Qtheor
The particle always moves at d c

. p f .g
its final settling velocity.

This settling velocity (Vc) is


proportional to the g force.

Problem:
A laboratory tubular-bowl centrifuge
has the following dimensions, with
respect to Figure 19.28, and operating
conditions: bowl speed 800 rps, R0 =
0.875 inch, R1= 0.65 in., and bowl
length = L = 4.5 inches. When used to
remove E. coli cells from the following
fermentation broth, a satisfactory
volumetric feed capacity of the
3
Broth:
f = 1.01
and is=
1.02 x 10-3 kg/m-s
centrifuge,
Q, ofg/cm
0.11 gpm
achieved.
E. coli: smallest diameter, dp,min = 0.7 mm and p = 1.04
g/cm3
Assuming the applicability of Stokes law, estimate the

Compute the sigma factor for the laboratory


centrifuge from using the given dimensions
and operating conditions.
The rotation rate, v, in radians/s=2(3.14)
(800)=5,030 s-1.

l R0 2 R12 vg 2
g ln R0 / R1

Solids-retaining Disc Centrifuge


Appropriate for liquid-solid or liquid-liquid
separations where the solids content is
less than about 1% by volume
For liquid-solid separations, the solids
that accumulate on the bowl wall are
recovered when the rotor capacity is
reached and the centrifuge is stopped
Removable baskets are
incorporated into
some designs to facilitate solids
Recovery of two liquid streams
removal
can be achieved by positioning
exit
Ports at different radial distances
as dictated by the relative
concentration of the liquids

Intermittent solids ejecting


disc centrifuge
Suitable for processing samples
with solids contents to about 15%
by volume
Solids or sludge that accumulate
on the bowl wall are
intermittently discharged through
a hydraulically activated
peripheral opening
Laboratory models to 18 cm
diameter and industrial
units to 60 cm
Industrial centrifuges
capable of throughputs in
excess of 100 m3 h-1

Bowl section of a self-cleaning disc stack centrifuge indicating


direction of fluid flow and ejection of sedimented solids through
passages controlled with hydraulically operated pistons

Discharge is intermittent
Nozzle machines
allow for
continuous
discharge of solids
through throttled
nozzles

Feed
Discharge
pump

Discharg
e

Timing unit

Solid bowl
machines without
solid discharge
mechanisms
require manual Annular
cleaning from time
piston
to time depending
upon feedstock

Photoce
ll

Discs

Sediment holding
space
Solids ejection
ports

Closing
chamber

Opening
chamber

Drain hole
Operating water

Continuous solids ejecting disc centrifuge


Solids contents ranging from 5 to
30% by volume
Solids are continuously
discharged via backward-facing
orifices
Newer designs discharge to an
internal chamber where the
discharge is
pumped out as a product stream
Industrial units are available
to 200 m3 h-1 throughput
capacity, elevated
temperature (<200oC) or
pressure (7 bar) capability,
and particle removal to 0.1

ormance analysis of disc type centrif

jective: To find the location of a given particle

Consider a particle at position


(x, y)
he velocity in the x direction is due to
nvection and sedimentation

dx
v0 v sin
dt
Average

Q
v0
f ( y)

n(2 rl )

x
R1

convective
velocity

The volume of v0 averaged over y


must equal the convective velocity

R0

Characteristics of v0
Much larger than
vsin
Function of radius

ormance analysis of disc type centrif

1
Q
v0 dy

l0
n
(2

rl
)

erforming integration we get


l

1
f ( y )dy 1

l0

x
R1

ain considering that the convective velocity


much greater than that of sedimentation

dx
v0 v sin v0
dt

f ( y)

n(2 rl )

R0

ormance analysis of disc type centri

he velocity in the y direction is due to


onvection and sedimentation

dy
v cos
dt
dy dy / dt
y

dx dx / dt
2 nlvg 2 r
2

r
cos

Qgf ( y )

In terms of R0

x
R1

R0

nlv

r
dy
g
2

( R0 x sin ) cos

dx Qgf ( y ) This describes the trajectory of the particle

between the discs

ormance analysis of disc type centri


particles which are most difficult to capture

ese particles enter at the outer edge of the discs where


0 and y=0

ey are captured at the inner edge of the discs at


and x=(R0-R1)/sin

er capture they and other particles are


y
ced along the disc surface to the outer
ge, where they are discharged.

x
R1

2 n 2

3
3
Q vg
( R0 R1 ) cot vg []
3g

R0

h the cases the quantity in square brackets has dimensions of (length)


ntially the term is dependent on the geometry of the centrifuge

Horizontal continuous-conveyer
centrifuge
Integrate an active mechanical solids discharge mechanism in an
imperforate bowl for the continuous processing of larger sample
volumes
The solids-discharge mechanism: A helical screw turning at a
slightly slower rate than the rotor
Capable of very high throughput, up to 300 000 L h-1

Basket type filtering


centrifuge
Combination of a centrifuge
and a filter with a rapidly
rotating perforated basket
Suspension is fed along the axis of the bowl and solids
accumulate on the wall basket

Liquid flows under centrifugal force through the cake which


accumulates on the basket wall and out through the
perforations in the wall
sed to wash accumulated
ake solids in filtration
Drainage number

d (G )1/ 2

Higher drainage
numbers
correspond to more

The theoretical sizing of a


centrifugal separator
Viscous drag is determining the particle
movement.
The flow in disk bowls between the disks
is laminar and symmetrical.
The liquid rotates at the same speed as
the bowl
The particle concentration is low (no
hindered settling)
The particle always moves at its final
settling velocity.
This settling velocity (Vc) is proportional to

Equivalent time
To assess the approximate properties of a
particle type to be separated, define a
dimensionless acceleration G

2R
G
g

This dimensionless unit is measured in terms of gs


(multiples of earths acceleration)

A rough approximation of the difficulty of a


2
separation by centrifugation isthe
R product of
t
the dimensionless acceleration Gt
(Gt )1
g
the time required for separation
Determination by
Centrifuging samples for various times until a constant
PCV is reached
The equivalent time is calculated as the product of G and
the time required for reaching the constant PCV

For scale up of centrifugation we can assume


constant equivalent time

(Gt ) 2

Typical equivalent time


values
System

Equivalent time
(sec)

Eukaryotic cells

0.3 x 106

Protein
precipitates
Bacteria

9 x 106

Ribosomes

1100 x 106

18 x 106

Problem: Scale-up based on


equivalent time
If bacterial cell debris has Gt = 54 x 106 s, how large
must be the centrifuge bowl and what centrifuge will
be needed to effect a full sedimentation in reasonable
amount of time?

R amount of time as 2 hours and


Assume the reasonable
Gt
t
0.5
the bowl radius as 10gcm.
m

6
0.5
54

10
s 9.81 2

Gtg
s

We know that

Rt
0.05m 2(3600) s

his speed can be easily achieved in


Solving for we get
production scale tubular centrifuge
rad
rev
60s
1213
1

11,590rpm
s
2 rad min

Characteristics of Separator Types

Coagulants and
flocculants
Metal salts
especially of aluminium or ferric iron

Natural flocculants

Starch, Gums, Tannin, Alginic acid, Sugar/sugar acid polymers,


Polyglucosamine (chitosan)

Synthetic flocculants
Polyacrylamides, Polyamines/imines, Cellulose
derivatives (e.g. carboxymethyl cellulose),
Polydiallydimethyl ammonium chloride

Chilling temperatures below 20oC, particularly


yeast cells
pH adjustment in range 3-6
Concentration
increases particle concentration, increasing collision

Problem: Complete recovery of bacterial


cells in a tubular bowl centrifuge
For complete recovery of bacterial cells from a
fermentation broth with a pilot plant scale tubular
centrifuge.
It has been already determined that the cells are
approximately spherical with a radius of 0.5 m and
have density of 1.1 g.cm-3
The
The
The
The

speed of the centrifuge is 5000 rpm


bowl diameter is 10 cm
bowl length is 100 cm
outlet opening of the bowl has a diameter of 4 cm

Estimate the maximum flow rate of the fermentation

Problem: Tubular centrifugation of E.coli


A bowl centrifuge is used to concentrate a suspension
of E.coli prior to cell disruption.
The bowl of this unit has an inside radius of 12.7 cm
and a length of 73 cm. the speed of the bowl is 16000
rpm.
The volumetric capacity is 200 litres/hr. Under these
conditons the centrifuge works well.
a) Calculate the settling velocity vg for the cells
b)After disruption the diameter of the debris is about
one half of the original cell diameter and the viscosity
is increased four times. Estimate the volumetric

Problem: Disc centrifugation of chlorella


Chlorella cells are being cultivated in open ponds. We
plan to harvest the biomass by passing the dilute
stream of cells through an available disc bowl
centrifuge.
The settling velocity vg for these cells has been
measured as 1.04 x 10-4 cm.s-1.
The centrifuge has 80 discs with an angle of 40o
Outer radius of 15.7 cm. Inner radius of 6 cm.
We plan to operate the centrifuge at 600 rpm.
Estimate the volumetric capacity Q for this centrifuge.

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