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CENTRIFUGATION

• Sedimentation and centrifugation


Sedimentation
 When a suspension is allowed to stand, the denser
solids slowly settle under the influence of gravity.
Centrifugation
 A settling process that is accelerated with a centrifugal
field.
Introduction (2/8)

• Comparison between filtration and centrifugation:

Feature Filtration Centrifugation


Separation principal Particle size Density
Employment Removal of Used when
insolubles filtration is
which are ineffective
dilute, large
and rigid
Product obtained Dry cake A paste or a more
concentrated
suspension
Expense of equipment Less More
Introduction (3/8)

• Separation cost for recovering whole cells or cell debris:

Ultrafiltration
more
economical

Centrifugation
more
economical

Ultrafiltration

Centrifugation
Introduction (4/8)

• Schematic presentation of a laboratory centrifuge:


Introduction (5/8)
• Care of centrifuges:
(1) Avoid imbalance in the rotor, which may be caused by:
a. Tube cracking during the run
* Conventional glass (Pyrex) centrifuge tubes
withstand only 3-4000 g.
 Use centrifuge tubes made from
polypropylene or polycarbonate.
b. Misbalance of the tubes in the first place
 Small tubes—balanced by volume by eye; large
tubes (> 200 mL)—should be weighed.
(2) Any spillage should be immediately rinsed away.
 Avoid corrosion of centrifuge rotors.
(3) Do not use the machine at top speed constantly.
Introduction (6/8)

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Introduction (7/8)

 2r
* Relative Centrifugal Force, RCF =
g

2  min 
1 rpm =  60 s  = 0.1047 s -1

min

g = 980 cm/s2
r: in cm
2
 0.1047 s 
2
-1
(rpm)   (r cm)
RCF =  rpm 
= 1.119  10 -5
(rpm) 2
(r )
2
980 cm/s

 Often an average RCF is determined using a value for r


midway between the top and bottom of the sample
container.
Introduction (8/8)

ravg = 7 cm
20,000 rpm  
RCF = 31,000
(centrifugal force = 31,000  g)
FORCES DEVELOPED IN CENTRIFUGAL
SEPARATION
The acceleration from a centrifugal force: a = 2r
where  = angular velocity, rad/s
r = radial distance from center of rotation
d2
Settling by gravity force: v g = ( s - )g
18

d2
v
Settling in centrifuges:  = (  -  ) 2
r
18
s
FORCES DEVELOPED IN CENTRIFUGAL SEPARATION (2/3)

• Gravitational sedimentation is too slow to be practical


for bacteria, and conventional centrifugation is too slow
for protein macromolecules.

__________
[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 m and a density of 1.05 g/cm3. The fluid has
physical 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:
dr d 2 r2 d2
v = = (  s -  ) 2 r or ln = (  s -  ) 2 t
dt 18 r1 18

(To be continued)
Example: laboratory bottle centrifuge

Solution (cont’d):
t = 0, r = 3 cm; t = ?, r = 10 cm
r2 d2
ln = (  s -  ) 2t
r1 18

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;
500  2
 = 500 rpm = = 52.3 rad/s
60
10 (8.0  10 -4 ) 2
ln =  (1.05 - 1)  (52.3) 2  t
3 18  0.01

 t = 2467 s = 41.3 min


#
FORCES DEVELOPED IN CENTRIFUGAL SEPARATION (3/3)

* Sedimentation Coefficient, s
“The velocity of a particle through a viscous medium
is usually proportional to the accelerating field.”

v = s 2 r

d2 d2
v = (  s -  ) 2 r  s= ( s -  )
18 18

Unit of s: svedberg (S; 1 S = 10-13 second)


 Svedberg: the inventor of ultracentrifuge
[Example] Estimate the time it would take to completely
clarify a suspension of 70 S ribosomes 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:
t 5
dr 1 dr
= s 2 r   dt = s 2 4 r
v =
dt 0

1 5 0.223
t= ln = = 29080 s = 8.1 h
s rev 2 1 min 
2

(70  10 s) 10000 min


2
4 -13
  
 rev 60 s 
#
TUBULAR BOWL CENTRIFUGE
• Suspension is usually fed through the
bottom, and clarified liquid is removed
from the top.
• Solid deposits on the bowl’s wall as a thick
paste.
• The suspension can be fed until solid loss in
the effluent becomes prohibitive.
• An intermittent operation.
TUBULAR BOWL CENTRIFUGE (2/6)

Assume that a particle is located at a distance z from the


bottom of the centrifuge and at a position r from the axis of
rotation. This particle is moving in both the z and r
directions.
TUBULAR BOWL CENTRIFUGE (3/6)

The movement of the particle in the z


direction (due to the convection of the
feed flow):
dz Q
=
dt  ( R02 - R12 )

where Q = the volumetric flow rate


R1 = the distance of liquid interface
from the axis of rotation
The movement of the particle in the r direction:
dr d 2
= (  s -  ) 2 r
dt 18
d2  2r 
vg = ( s - )g 
dr
= v g  
18 dt  g 
TUBULAR BOWL CENTRIFUGE (4/6)

dz Q dr  2r 
= ; = v g  
dt  ( R02 - R12 ) dt  g 

The trajectory of a particle in the


centrifuge:
dr dr / dt   2 r   ( R02 - R12 )
= = v g  
dz dz / dt  g  Q

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


at z = 0, r = R1) and do not reach R0 until at z = 

R 0 v g   ( R - R )
2 2 2 ( R02 - R12 )v g  2
ln = 0 1
or Q=
R1 g Q g ln(R0 / R1 )
TUBULAR BOWL CENTRIFUGE (5/6)

( R02 - R12 )v g  2


Q=
g ln(R0 / R1 )

For R0 and R1 being approximately equal,


R02 - R12 ( R0 + R1 )( R0 - R1 ) ( R0 + R1 )( R0 - R1 )
= = = R1 ( R0 + R1 ) = 2 R 2
ln( R0 / R1 ) ln[1 + ( R0 - R1 ) / R1 ] ( R0 - R1 ) / R1

1 2 1 3 1 4
Note: ln(1 + x) = x - x + x - x + 
2 3 4
 2R 2 2 
 Q = v g   = v g ()
 g 
Note: vg is a function only of the particles themselves, and 
is a function only of the particular centrifuge.
TUBULAR BOWL CENTRIFUGE (6/6)

* Continuous tubular bowl


centrifuge for separation of
two liquids:
An internal baffle provides a
separate passage adjacent to
the bowl wall to conduct the
heavier-phase liquid to a
different discharge elevation.
[Example] A bowl centrifuge is used to concentrate a
suspension of Escherichia coli prior to cell disruption. The
bowl of this unit has an inside radius of 12.7 cm and a
length of 73.0 cm. The speed of the bowl is 16,000 rpm and
the volumetric capacity is 200 L/h. Under these conditions,
this centrifuge works well. (a) Calculate the settling
velocity vg for 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:
 2R 2 2  Qg
Q = v g   or v g =
 g  2R 
2 2

(To be continued)
[Example] Analysis of bowl centrifuge
(a) Calculate the settling velocity vg for the cells.
(b) Estimate the volumetric capacity of this same centrifuge for cell
debris.
Solution: Qg
vg =
2R 2 2
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  10-7 cm/s
Q2 v g 2  v g 2
Using the same centrifuge, = =
Q1 v g1 v g1

d 2 Q d 2
/  d 2
/ d 2
(1 / 2) 2
1
vg = ( s - )g 
2
= 2 2
= 2 1
= =
18 Q1 d 12 / 1  2 / 1 4 16
#
[Example] Beer with a specific gravity of 1.042 and a
viscosity of 1.4  10-3 N-s/m2 contains 1.5% solids, which
have a density of 1160 kg/m3. It is clarified at a rate of 240
L/h in a bowl centrifuge, which has an operating volume of
0.09 m3 and a speed of 10,000 rev/min. The bowl has a
radius of 5.5 cm and is fitted with a 4-cm outlet. Calculate
the effect on feed rate of an increase in bowl speed to 15,000
rev/min and the minimum particle size that can be removed
at the higher speed.

Solution:
( R02 - R12 )v g  2  2 (  s -  )d 2
Q= = [( R02 - R12 )]
g ln( R0 / R1 ) 18[ln( R0 / R1 )]
All conditions except the bowl speed remain the same.
Q2  22
= 2
Q1  1
(To be continued)
[Example] Beer with a specific gravity of 1.042 and a viscosity of 1.4 
10-3 N-s/m2 contains 1.5% solids, which have a density of 1160 kg/m3. It
is clarified at a rate of 240 L/h in a bowl centrifuge, which has an
operating volume of 0.09 m3 and a speed of 10,000 rev/min. The bowl
has a radius of 5.5 cm and is fitted with a 4-cm outlet.
Calculate: when  = 15,000 rev/min, Q = ? d = ?
Solution (cont’d):
 2 (  s -  )d 2
Q= [( R02 - R12 )]
18[ln( R0 / R1 )]

Q2  22 Q2 (15000) 2
= 2  =
Q1  1 240 (10000) 2

 m3   h  -4
 Q2 = 540 L/h  =  3
   1.5 10 m /s
1000 L   3600 s 
(To be continued)
[Example] Beer with a specific gravity of 1.042 and a viscosity of 1.4 
10-3 N-s/m2 contains 1.5% solids, which have a density of 1160 kg/m3. It
is clarified at a rate of 240 L/h in a bowl centrifuge, which has an
operating volume of 0.09 m3 and a speed of 10,000 rev/min. The bowl
has a radius of 5.5 cm and is fitted with a 4-cm outlet.
Calculate: when  = 15,000 rev/min, Q = ? d = ?
Solution (cont’d):
15000  2
= = 1570 s -1
60
Operating volume = [( R0 - R1 )] = 0.09 m
2 2 3

 2 (  s -  )d 2
Q= [( R02 - R12 )]
18[ln( R0 / R1 )]

-4 (1570) 2 (1160 - 1042)d 2


 1.5  10 = -3
[0.09]
18(1.4  10 ) ln( 5.5 / 4)
 d = 2.14  10-7 m #
SEPARATION OF LIQUIDS BY CENTRIFUGATION
 A common operation in the food and other industries.
* Example: the dairy industry, in which the emulsion of
milk is separated into skim milk and cream.
SEPARATION OF LIQUIDS BY CENTRIFUGATION (2/3)

The differential force across a


thickness dr is:
dF = r2dm
dF
dm =  [(2rdr )] and dP =
2r
r 2 [(2rdr)]
- dP = =  2 rdr
2r

Integration between r1 and r2:

 2
P1 - P2 =
2
(r
2
2
- r12 )
SEPARATION OF LIQUIDS BY CENTRIFUGATION (3/3)

 2
P1 - P2 =
2
(r 2
2
- r12 )
At the liquid-liquid interface,
Pressure exerted by the light
phase of thickness (r2 - r1)
= Pressure exerted by the heavy
phase of thickness (r2 - r4)
H 2  L 2

2
(r
2
2
- r42 =) 2
(r
2
2
- r12 )
 r 2
-  r 2

 r22 = H 4 L 1

H - L

* The interface at r2 must be located at a radius smaller


than r3.
[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/m3 and that of the aqueous
phase is 980.3 kg/m3. The radius for overflow of the light
liquid has been set at 10.160 mm and the outlet for the
heavy liquid at 10.414 mm. Calculate the location of the
interface in the centrifuge.

Solution:
 r 2
-  r 2
r22 = H 4 L 1

H - L
980.3(10.414 ) 2
- 919.5(10.160) 2
 r22 =
980.3 - 919.5

 r2 = 13.75 mm
#
DISK CENTRIFUGE
DISK CENTRIFUGE (2/14)

• A short, wide bowl 8 to 20 in.


in diameter turns on a vertical
axis. 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 liquid
enters the bowl at the bottom,
flows into the channels, and
upward past the disks.
DISK CENTRIFUGE (3/14)

• The operation can be made continuous.


___

___

____
Collection of solid:
DISK CENTRIFUGE (6/14)

• A properly operated disc centrifuge should separate


99% of the solids from the liquid stream and produce
an 80-90% 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 the
diameter of the particle.
d2
Q = vg  ; vg = ( s -  )g
18
* Cell debris (particle size  0.5 m) can be
separated with flow rates of 300-500 L/h.
DISK CENTRIFUGE (7/14)

• In actual operation, the desired separation is achieved by


empirically determining:

(a) The flow rate of feed that yields a clarified


supernatant liquid
(b) The time interval between solid discharges that will
minimize liquid loss while still allowing the solids to
flow
 Discharge periods are on the order of 0.1 s.
DISK CENTRIFUGE (8/14)

Consider a particle located


at position (x, y), where x is
the distance from the edge
of the outer disks along the
gap between the disk, and
y is the distance normal to
the lower disk. Liquid is
fed into the centrifuge so
that it flows upward
through the gap between
the disks, entering at R0
and leaving at R1.
DISK CENTRIFUGE (9/14)

The velocity of the particle in the x direction is:


dx
= v 0 - v sin 
dt
where v0 is the convective liquid velocity, and v is the
particle’s velocity under centrifugation.
DISK CENTRIFUGE (10/14)

There are three important characteristics of v0:


(1) Under most conditions, v0 >> vsin.
(2) v0 is a function of radius.
(3) v0 is a function of y.
dx  Q 
= v0 =   f ( y)
dt  n(2r) 

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
DISK CENTRIFUGE (11/14)

dx  Q 
= v0 =   f ( y)
dt  n(2r) 

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


 
1 1 Qf ( y )
Q = n(2r)   v 0 dy = n(2r)   dy
0  0 n(2r)

1

0 f ( y )dy = 1
DISK CENTRIFUGE (12/14)

dx  Q 
= v0 =   f ( y)
dt  n(2r) 

The velocity of the particle in the y direction is:


dy   2r 
= v cos = v g   cos
dt  g 
The trajectory of a particle between the disks of this
centrifuge is:
dy dy / dt  2nv g   2
2

= =  r cos 
dx dx / dt  Qgf ( y ) 
DISK CENTRIFUGE (13/14)

dy dy / dt  2nv g   2
2

= =  r cos 
r = R0 - x sin  dx dx / dt  Qgf ( y ) 

r = R0 - x sin 

dy  2nv g  
2

 =  ( R0 - x sin  ) cos 
2

dx  Qgf ( y ) 
DISK CENTRIFUGE (14/14)

dy  2n v  2

=  ( R0 - x sin  ) cos 
g 2

dx  Qgf ( y ) 

1
r = R0 - x sin  0 f ( y )dy = 1

Integration for those particles that 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.)

 2n 2 3 
 Q = vg  ( R0 - R1 ) cot  = v g ()
3

 3g 
[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 vg for these cells has been measured as
1.07  10-4 cm/s. The centrifuge has 80 discs with an angle of
40, 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 capacity Q for this centrifuge.

Solution:  2n 2 3 
Q = vg  ( R0 - R1 ) cot 
3

 3g 
Data: vg = 1.07  10-4 cm/s; n = 80; R0 = 15.7 cm; R1 = 6 cm;  = 40; g =
980 cm/s2

6000  2
= = 628 rad/s  Q = 3.14  104 cm3/s = 31.4 L/s
60
#
SCALEUP OF CENTRIFUGATION
 Use laboratory data to predict performance of
commercially available centrifuges.
• Commercially available centrifuges are designed on a
mechanical basis and 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)

• Scaleup of centrifugation based on the equivalent time Gt


Gt: a measurement of the difficulty of a given separation
 2R
Gt = t
g
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 Gt is determined, a large-scale


centrifuge that has a similar Gt should be considered.
* This approach must be regarded as only a crude
approximation.
SCALEUP OF CENTRIFUGATION (3/5)

Values of Gt for various solids:


[Example] It has been shown that bacterial cell debris
has Gt = 54  106 s. For a centrifuge bowl of 10 cm in
diameter, find the centrifuge speed if a full
sedimentation in 2 h is required.
Solution:
 R
2  2
(5)
Gt = t  54  106 =  (2  3600)
g 980

 
1 rev 
60 s
  = 1212 rad/s     = 11,580 rpm
 2 rad   min 
#
SCALEUP OF CENTRIFUGATION (4/5)

• Scaleup of centrifugation using the  factor (Q = vg)


 Scaleup involves choosing a centrifuge that has
the required  value to meet the process
requirements of vg and Q.

* The value of  is really the area of a gravitational


settler that will have the same sedimentation
characteristics as the centrifuge for the same feed
rate.
SCALEUP OF CENTRIFUGATION (5/5)

• Scaleup of centrifugation using the  factor (Q = vg)

* Scaleup from a laboratory test of Q1 and 1 to Q2


using similar type and geometry centrifuges:
Q1 Q2
=
1  2

* Scaleup if different centrifuges are used:


Q1 Q2
=
E1  1 E 2  2

E is the efficiency of a centrifuge, which is determined


experimentally.
[Example] The old process for recovering starch particles
from a slurry of starch and gluten involved a gravitational
settling procedure in which the slurry was fed to one end of
a table where the starch particles settled and remained in
the table and starch-free liquid was discharged from the
opposite end of the table. We have been asked to evaluate a
process improvement involving the use of continuous
centrifuges. It has been reported that a starch table with
the dimensions of 2 ft wide and 120 ft long can handle a
slurry feed rate of 2 gal/min. The slurry has a viscosity of
10-3 kg/m-s and a density difference of 100 kg/m3. The
centrifuge has a  value of 31,500 m2.
(a) Calculate the effective diameter of the starch particles.
(b) Estimate the centrifuge throughput, assuming that you
can operate at 50% of the theoretical maximum.
(To be continued)
[Example] Recovery of starch particles.
 = 10-3 kg/m-s; s –  = 100 kg/m3
(a) Calculate the effective diameter of the starch particles.

Solution:

A starch table with the dimensions of 2 ft wide and 120 ft long can
handle a slurry feed rate of 2 gal/min.

2 gal/min  ft 3   m   min  -6
v =
 g 2  120 ft 2  7.48 gal   3.28 ft   60 s  = 5.66  10 m/s
   

d2 d 2
vg = (  s -  ) g  5.66  10 -6 = (100)(9.8)
18 -3
18  (10 )
 d = 1.02  10-5 m
(To be continued)
[Example] Recovery of starch particles. The centrifuge has a  value of
31,500 m2. (b) Estimate the centrifuge throughput, assuming that you
can operate at 50% of the theoretical maximum.

Solution (cont’d):
vg = 5.66 10 -6 m/s

Q at 50% of the theoretical maximum


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

m3 1000 L   7.48 gal   60 s 


= 0.089  m 3   28.32 L   min  = 1410 gal/min
s

#
[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 min at
2000 rpm. In the lab centrifuge, the inner radius of the
solution is 5 cm and the bottle tip radius is 15 cm. The cell
suspension contains only 7% by volume of cells. We are
asked to recommend the size and type of centrifuge for
separating 10 m3 of this suspension per day.
Solution: Q = vg
dr  r 
2 R0
dr vg 2 t

= v g    R r = g  dt
dt  g  1 0

R0 v g  t
2
g ln( R0 / R1 )
 ln = or v =
 2t
g (To be continued)
R1 g
[Example] Recommend the size and type of centrifuge for separating
10 m3 of a yeast suspension per day.

Solution (cont’d):
g ln( R0 / R1 )
vg =
 2t

Data: R1 = 5 cm; R0 = 15 cm; t = 30 min;  = 2000 rpm

 vg = 1.36  10-5 cm/s

Q 10 m 3 / day
= = = 851 m 2

v g 1.36  10 -5 cm/s #

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


centrifuges, while no safety factor is needed for tubular
bowl centrifuges.
[Example] We want to centrifuge chlorella cells using an
available disc bowl centrifuge operated at 6000 rpm. The
centrifuge has 80 discs with an angle of 40, an outer radius
of 15.7 cm, and an inner radius of 6 cm. The cell suspension
has a viscosity of 1 cp and a density difference of 0.1 g/cm3.
The effective diameter of chlorella cells is 4.3  10-4 cm.
Assume the efficiency of the disc centrifuge is 0.5; estimate
the throughput.
Solution:  g 
 poise : 
 cm - s 
d2 (4.3  10 -4 ) 2
vg = ( s -  )g = (0.1)(980) = 1.01  10 - 4 cm/s
18 18(0.01)
 2   min 
 = 6000 rev/min    = 628 s -1

 rev   60 s 
 2n 2 3 
Q = vg  ( R0 - R13 ) cot  E  = 14,820 cm3/s
 3g  #
SCROLL TYPE OF DECANTING CENTRIFUGE
Horizontal Type

 * An internal scroll conveyor is used to move the decanted


solid out of the machine.
* Centrifugal force: 500-6,000 g
* Scroll Decanting
Centrifuge: Vertical
Type (2/2)
ULTRACENTRIFUGE
 The term “ultracentrifuge” was originally applied by T.
Svedberg to 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-force


centrifuge (up to 75,000 rpm, with RCF values up to
500,000  g).
ULTRACENTRIFUGE (2/3)
ULTRACENTRIFUGE (3/3)
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
Classification Equipment Subclassification
Major function Operation Classification
Classification Equipment Subclassification
CENTRIFUGAL EXTRACTOR
CENTRIFUGAL EXTRACTOR (2/2)

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