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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
– solid–liquid separation
– liquid–liquid 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

2

Buoyancy force
Fb  mM g  V p  M g

mM = the mass of the fluid
medium displaced
Vp = the volume of the
particle
ρM = 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
ρM = the density of the medium
(g.cm-3)
ρP = 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, η as described for a
spherical particle by Stokes’ equation

 dx
Ff  6 r  
 dt
η = 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).

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

which concentration gradient tends to concentrate particles .Effect of Diffusion Fick’s 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.

Sedimentation in a Centrifugal Field A particle moving in a circular path continuously experiences a centrifugal force. The centrifugal force may be expressed as Fc  ma  m x 2 m = the particle mass (g). Fc. a = the acceleration (cm. This force acts in the plane described by the circular path and is directed away from the axis of rotation.rpm/60) x = the radial distance from the axis of rotation to the particle (cm) .s-2) ω = the angular velocity (radians s-1 π.

Relative centrifugal force (RCF) Ratio of acceleration of the centrifugal field to that of acceleration owing to the earth’s gravity Fc RCF   Fg 2 m   x  mg   2   x g Alternatively RCF is given by RCF  1.rpm/60). a = the acceleration (cm. . x = the radial distance from the axis of rotation to the particle (cm). ω = the angular velocity (radians s-1 2π.119 10 5  rpm  2 x m = the particle mass (g).s-2).

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 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. 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 . d and particle velocity.

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. • Measure of the sedimentation velocity per unit of centrifugal force . 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 ω2x  dx   2r 2      dt P M  Sr  2  9   x – expressed in terms of the sedimentation coefficient. S.

Sedimentation Coefficient • The sedimentation coefficient has the dimensions of seconds – expressed in Svedberg units equal to 10-13 s • Sedimentation coefficient is dependent on S – the particle being separated20.M   P   M  20.W   P  T . M  . w – the centrifugal force – the properties of the sedimentation medium.  • Useful to compare sedimentation coefficients obtained – under differing conditions – sedimentation media by reference ST . MT .

53 10  ln  rmax  rmin  / rpm 11 2 . is a function of rotor design and is a constant for a given rotor.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. • 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.

to a second rotor of differing geometry by solving for t2 in the relation . t1.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  2 k-Factors are also useful when switching from a rotor with a known pelleting time.

02 g/ml and a diameter of 150 μm. A 50 litre stirred tank is used to cultivate cells grown on microcarriers to produce a viral vaccine. These cell laden beads or “microcarriers” have a density of 1. the carrier-free fluid has density of 1 g/ml and a viscosity of 1. After growth.em: Separating cells growing on a suppo Animal cells can be cultivated on the external surface of dextran beads.1 cP. a) Estimate the settling time to reach the velocity . 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 stirring is stopped and are allowed to settle.

022cm / sec)1g / cm3) Re    0.015cm)(0.03  (0.3cm .sec)  2 V d l Hence the use of Stoke’s equation is justified 4 2  l  To calculate the liquid height from tank volume 3 3   l  50  10 cm  4  1.022cm.5 l  52.(a) Using the equation for terminal velocity v Substituting the values we get 2 2 d       P M  x 18 v  0.011g / cm.s 1 du  Re  1 okes law is applicable if the condition is satisfied that  du  (0.

The terminal velocity of the particle can be made use of to calculate the settling time t = l/vg = 52.6 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 g 3 dv d3  P  M  6 18v g 2 d  P  M  .3 cm/0.022 cm/sec = 39.

02 g / cm3 )   2.sec) nce our settling time is 40 minutes we easily meet this criter .015cm) 2 (0.dvg g 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 (0.27 105 sec 18(0.011g / cm.

The centrifuge is to be operated at 500 rpm. . The fluid has physical properties close to those of pure water.05 g/ml.0 μm and a density of 1. with a diameter of 8. and the distance from the bottom of the cylinder to that axis is 10 cm.oblem: Centrifugation of yeast cells A laboratory bottle centrifuge consists of a number of cylinders rotated perpendicular to the axis of rotation. The yeast cells can be assumed to be spherical. During centrifugation the distance between the surface of liquid and the axis of rotation is 3 cm.

r = 3 cm.01 g .05     1 1 3  3 cm 18(0. we find r  d2 2 ln   (  s   )  t  18  3cm  Substituting the values. t = 0. cm .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. we get  500  2 2 (8 104 cm) 2  g  10cm ln  0.sec cm 60sec       t  2500sec . Integrating the initial equation.

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 .

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.h-1 Centrifugal forces ranging up to 62000g.models are available with Laboratory Diameters of 4.8 m Holding capacities up to 12 kg Throughput rates of 250 m3 h-1 Centifugal forces ranging up to 20000 g. .ubular bowl centrifuge Utilize a vertically mounted.5 cm Throughput rates of 150 L.

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

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 2   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  R   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 Q  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 [ ]  g   ...

.

 p   f .g its final settling velocity. The equation for critical diameter become 1 The flow in disk bowls 2 between the disks is laminar  18.r  The liquid rotates at the same   speed as the bowl 1 The particle concentration is 2   low (no hindered settling).Qtheor The particle always moves at d c     .he Generalized Σ Formula The most-used quantity to characterize centrifuges. Assumptions • • • • • • 2 lR   g Viscous drag is determining the particle movement. 18. the Σ concept 2 2 Qtheor  vg .     . Where.   This settling velocity (Vc) is proportional to the g force. . 2 2   p   f V .Q  Se theor and symmetrical.  dc   . . .

estimate the .28.02 x 10-3 kg/m-s centrifuge. and operating conditions: bowl speed 800 rps. dp. When used to remove E.5 inches.875 inch.min = 0.65 in. R0 = 0.Problem: A laboratory tubular-bowl centrifuge has the following dimensions. a satisfactory volumetric feed capacity of the 3 Broth: ρf = 1.7 mm and ρp = 1. R1= 0. with respect to Figure 19. coli cells from the following fermentation broth..04 g/cm3 Assuming the applicability of Stokes’ law.11 gpm achieved.01 and μis= 1. Q. E. ofg/cm 0. coli: smallest diameter. and bowl length = L = 4.

in radians/s=2(3.030 s-1.Compute the sigma factor for the laboratory centrifuge from using the given dimensions and operating conditions. The rotation rate.14) (800)=5. v. Q  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 .

1 . and particle removal to 0. elevated temperature (<200oC) or pressure (7 bar) capability.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.

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 ) θ y x R1 convective velocity The volume of v0 averaged over y must equal the convective velocity R0 Characteristics of v0 Much larger than vωsinθ Function of radius .ormance analysis of disc type centrif ω jective: To find the location of a given particle Consider a particle at position (x.

ormance analysis of disc type centrif ω  1 Q  v0 dy     l0 n (2  rl )   l θ erforming integration we get l 1 f ( y )dy  1  l0 y x R1 ain considering that the convective velocity much greater than that of sedimentation dx  v0  v sin   v0 dt  Q   f ( y)   n(2 rl ) R0 .

ormance analysis of disc type centri ω 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 θ x R1 R0 2  2  nlv  r dy g 2  ( R0  x sin ) cos     dx  Qgf ( y )  This describes the trajectory of the particle between the discs .

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 Σ has dimensions of (length) ntially the term Σ is dependent on the geometry of the centrifuge .ormance analysis of disc type centri particles which are most difficult to capture ese particles enter at the outer edge of the discs where ω 0 and y=0 θ ey are captured at the inner edge of the discs at and x=(R0-R1)/sinθ er capture they and other particles are y ced along the disc surface to the outer ge.

up to 300 000 L h-1 .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.

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 .

• This settling velocity (Vc) is proportional to .The theoretical sizing of a centrifugal separator • Viscous drag is determining the particle movement. • 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. • The flow in disk bowls between the disks is laminar and symmetrical.

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 ‘g’s (multiples of earth’s acceleration) • A rough approximation of the difficulty of a 2 separation by centrifugation isthe 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 .

3 x 106 Protein precipitates Bacteria 9 x 106 Ribosomes 1100 x 106 18 x 106 .Typical equivalent time values System Equivalent time (sec) Eukaryotic cells 0.

05m  2(3600) s   his speed can be easily achieved in Solving for ω we get production scale tubular centrifuge rad rev 60s  1213 1   11.590rpm s 2 rad min . m   6 0.Problem: Scale-up based on equivalent time If bacterial cell debris has Gt = 54 x 106 s.5 54  10 s  9.5 the bowl radius as 10gcm. how large must be the centrifuge bowl and what centrifuge will be needed to effect a full sedimentation in reasonable amount of time? 2  R amount of time as 2 hours and Assume the reasonable Gt  t 0.81 2   Gtg s      We know that   Rt   0.

Characteristics of Separator Types .

carboxymethyl cellulose).Coagulants and flocculants • Metal salts – especially of aluminium or ferric iron • Natural flocculants • Starch. Polydiallydimethyl ammonium chloride • Chilling temperatures below 20oC. Polyamines/imines. Sugar/sugar acid polymers.g. Cellulose derivatives (e. increasing collision . Tannin. Alginic acid. Gums. particularly yeast cells • pH adjustment in range 3-6 • Concentration – increases particle concentration. Polyglucosamine (chitosan) • Synthetic flocculants – Polyacrylamides.

It has been already determined that the cells are approximately spherical with a radius of 0.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: 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.5 μm and have density of 1.1 g.

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. The bowl of this unit has an inside radius of 12.Problem: Tubular centrifugation of E. The volumetric capacity is 200 litres/hr.coli prior to cell disruption.7 cm and a length of 73 cm. Estimate the volumetric .coli A bowl centrifuge is used to concentrate a suspension of E. Under these conditons the centrifuge works well. the speed of the bowl is 16000 rpm.

Inner radius of 6 cm.Problem: Disc centrifugation of chlorella Chlorella cells are being cultivated in open ponds. The centrifuge has 80 discs with an angle of 40o Outer radius of 15. We plan to harvest the biomass by passing the dilute stream of cells through an available disc bowl centrifuge. .7 cm.s-1. We plan to operate the centrifuge at 600 rpm. The settling velocity vg for these cells has been measured as 1.04 x 10-4 cm. Estimate the volumetric capacity Q for this centrifuge.