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Batch Distillation

And
Plate Column and Packed Column Sizing

Er.. RAHUL CHAUDHARI


Er
Assistant Professor

Department of Chemical Engineering


Jaypee University of Engineering and Technology,
Guna, M.P.
BATCH DISTILLATION

A very common unit operation used in manufacturing of chemicals which


are produced in batch process.

Batch distillation is an unsteady-state process: the composition in the still


and the overheads changing as the batch is distilled.

Batch Distillation is carried out with or without using a rectification column.

Thus, it is divided in two types:

1) Simple Distillation
2) Batch Distillation with Rectification

1. Simple Distillation:
In batch distillation, the feed is charged to the still pot to which heat is
supplied.

As the mixture boils, it generates a vapor richer in the more volatile component.

As boiling continues concentration of MVC in the liquid decreases.

At the beginning, the condensate will be pretty rich in the more volatiles but
concentration of more volatiles will decrease in distillate as the condensate
keeps on accumulating in the receiver.

Following equation is applicable to the simple batch distillation:

F x F dx
ln x *
W w y x

F F 1 xF
ln ln
W W 1 xW
2. Batch Distillation with Rectification:

In this cases the whole of a batch is run into the boiler of the still and, on heating, the vapour is
passed into a fractionation column, as shown in above fig.

As observed from the above fig there is only rectification zone appears from the bottom to
top of the column hence, in batch distillation one has to only deal with one operating line
i.e. rectifying Section operating line.
As with continuous distillation, the composition of the top product depends
on the still composition, the number of plates in the column and on the reflux ratio
used.

When the still is operating, since the top product will be relatively rich in the more
volatile component, the liquid remaining in the still will become steadily weaker in
this component.

As a result, the purity of the top product will steadily fall.....

To get the constant overhead composition, the amount of reflux returned


to the column must be continuously increased throughout the run.

An alternate method of running a batch distillation is to fix the reflux ratio


constant and let the overhead product purity vary with time. Then stopping
the distillation when the amount of product or the average concentration
in the total product reaches a specified value.

The most preferred method from above two, is the


the constant overhead composition
with varying reflux .
Process Design for Binary Batch Rectification with
Constant Overhead composition.
composition

For a binary system, approximate but useful method is based on McCabe Thiele
graphical method.

For a multi-components system, Approximate FUG method and Rigorous Lewis Matheson
method can be the useful methods.

For Binary System:


1. Determine the minimum reflux ratio by using following equation,

LV
min
Rmin
1 L
Vmin

Where, (L / V ) min = Minimum internal reflux ratio or


Slope of operating line which passes through
either by touching point of inflection or point of
intersection of q-line and equilibrium line.

Alternatively,
Rmin can also be determine from the intercept of operating line which passes through
either by touching point of inflection or point of intersection of q-line and equilibrium line.
2. Determine the value of reflux ratio required for starting conditions.

3. Draw the operating line for starting of batch distillation.

4. Determine the number of theoretical stages required for the desired separation at the
Start of batch distillation.

5. Continue these calculations until, new value of xwi obtained, is equal to xB, where
xB is equal to mole fraction of more volatile component required in bottom product.

6. Time required for batch distillation rectification with constant overhead composition
can be calculated by Bogart equation,

xF
F ( x D xF ) dxw
x 1 L ( x x ) 2
V B
V D W

Where,
= Total time required in batch distillation with rectification in seconds.
F = Total moles of feed charged, kmol.
V = Molar flow rate of vapor phase, kmol/s.
L = Molar flow rate of liquid phase, kmol/s.
xD = Mole fraction of more volatile component in distillate.
xB = Mole fraction of more volatile component in bottom product or final residue.
xW = More fraction of more volatile component in liquid inside the still or reboiler
xF = Mole fraction of more volatile component in feed.
Bogart Equation can also be written as,

xF
F ( xD xF ) dxw
x 1 L
V Wi
V
( x D xWi ) 2

Where,
xWi = intermediate composition of more volatile component in liquid inside the still or reboiler.

7. The quantity of distillate at any time can be determined by using the following equation,

F ( xF xWi )
D F Wi
xD xWi
Where,
Wi = Moles of liquid in still at any time .

At the end of distillation, quantity of material distilled,

F ( xF xB )
D F Wi
xD xB
Heat to be supplied in the boiler to provide this reflux during the total distillation:

If the reflux ratio R is assumed to be adjusted continuously to keep the top


product at constant quality,

then at any moment the reflux ratio is given by R = dL/dD

During the course of the distillation, the total reflux liquor flowing down the
column is given by:
L R2

dL R dD
0 R1

To provide the reflux dL the removal of a quantity of heat equal to dL in the


condenser is required, where is the latent heat per mole,

Thus, the heat to be supplied in the boiler to provide this reflux during the total
distillation QR is,
L R2

Q R dL R dD
0 R1
Ten kilomoles of acetone has been pumped by mistake into a storage vessel of ethanol
containing 10 kilomoles of ethanol. It is decided to separate the mixture by batch
distillation. Ten mole % of alcohol in the top product and 12 mole % acetone in the bottom
product are acceptable. A column having six theoretical plates, a reboiler and a condenser
is available. The operation is to be carried out at essentially atmospheric pressure and the
reflux is to be returned at its bubble point. Calculate (a) the amounts of top and bottom
products. (b) What initial and final Reflux ratios should be used? (c) Determine the total
moles of vapor to be generated to achieve the separation. (d) If steam is supplied to the coils
in the still at such a rate that 6 kmol of vapor is generated per hour, calculate the time
required for distillation. The vapor-liquid equilibirum data for the acetone-ethanol system
are given below:

x 0.05 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00
y 0.16 0.25 0.42 0.51 0.6 0.67 0.72 0.79 0.87 0.93 1.00
Solution:
i) Do the overall material balance and obtained top and bottom products qty.
ii) Draw the equilibrium line on the x-y plane.
iii) Locate the point (xD, xD) where xD = 0.90.
iv) In each case, fit seven ideal stages between the operating line and the equilibrium line and
determine the bottom concentration, xW.
v) Using the (xD, xW) data as well as slope of the bunch of operating lines drawn, evaluate the
integral part of Bogarts equation graphically to get the total moles of vapor generated
during distillation.
Also see the example 8.15, page no. 483 in text book Introduction to Process
Engineering and Design by Bhatt and Thakore.
Stage efficiency analysis:

In general the overall efficiency will depend:

1) Geometry and design of contact stages.

2) Flow rates and patterns on the tray.

3) Composition and properties of vapour and


liquid streams.
Three principal definitions of efficiency are used:

1. Point efficiency (Murphree point efficiency).


2. Murphree plate efficiency.
3. Overall column efficiency.
Stage efficiency analysis:

Lin,xin Vout,yout
What are the sources of inefficiencies?

Lout,xout Vin,yin For this we need to look at what actually happens


on the tray

Local efficiency

yn yn 1 Actual separation
Emv *
yn yn 1 Separation that
would have been
achieved on an
ideal tray

Point efficiency
Stage efficiency analysis

stagnation points Depending on the location on the tray


the point efficiency will vary

The overall plate efficiency can


be characterized by the Murphree
plate efficiency:

Murphree plate efficiency uses avg. conc.


Thus by using avg. concentration we have,
high concentration low concentration
gradients yn yn 1
gradients
EmV *
yn yn 1

When both the vapour and liquid


phases are perfectly mixed the plate
efficiency is equal to the point EmV Emv
efficiency
The Murphree plate efficiency and point or local efficiency can be related
based on the extent of mixing of the liquid and vapor.

When both the vapour and liquid


phases are perfectly mixed the plate EmV Emv
efficiency is equal to the point
efficiency

When the liquid is in plug L mVEmv


flow and no axial mixing at all EmV exp 1
occurs in the liquid. mG L
Overall column efficiency: This is sometimes referred to as the overall plate
efficiency.
number of ideal stages
EO
number of real stages
It is sometimes used to determine the number of real stages.

For the idealised situation where the operating and equilibrium lines are straight,
the overall column efficiency and the Murphree plate efficiency are related by an
equation derived by Lewis,

mV
log 1 E mV 1
L
EO
mV
log
L
Prediction of plate efficiency:

OConnell (1946):

A quick estimate of the overall column efficiency can be obtained from the
correlation given by O'Connell,

EO 51 32.5 log( a a )
Where, a the molar average liquid viscosity, mNs/m2,
a - average relative volatility of the light key.
O'Connell gave a similar correlation for the plate efficiency of absorbers,

Where,

Appreciably lower plate efficiencies are obtained in absorption than in distillation.


Van Winkle (1972)
AIChE Method:
1 1 mV 1

ln 1 Emv N
G L N L

where m is the slope of the operating line and V and L the vapour and
liquid molar flow rates.

Ref: RC-6
Stage efficiency analysis

In general a number of
empirical correlations exist
that relate point and plate
efficiencies

Peclet number

Z L2 length of liquid
N Pe flow path

Detc
eddy diffusivity residence time of liquid
on the tray
Column Sizing for Absorption , Distillation, and Extraction:

The objective is to achieve an intimate contact between the phases and to


Ensure a rate of mass transfer.

A high degree of turbulent mixing to generate a large interfacial area of contact


leading to increase mass transfer coefficient.

Interfacial area is generated by passage of the gas in to the liquid through


perforations or openings. TRAY TOWERS/COLUMNS

Alternatively, interfacial area is created by spreading the liquid on the packing


surface. PACKED TOWERS/COLUMNS
Selection Criterion between tray tower and packed tower:

1. Pressure Drop: Packed tower generally provides low pressure drops, therefore for
high vacuum distillation, a packed tower is selected.

2. Tower Diameter: For very small tower diameter packed tower is preferred. With large
tower diameter, tray tower is preferred. With very small diameter (less than 150 mm),
fabrication of trays is difficult while with large diameter, liquid distribution is difficult in
the packed tower.

3. L/V Ratio: For handling higher ratio of liquid to vapor flow rate (L/V), packed tower are
preferred. But for low L/V ratio tray tower is selected. [Packed tower requires minimum
wetting rate to work efficiently. At low gas flow Rate plate columns are prone to weeping
and dumping]

4. Residence Time of liquid: Liquid hold up in tray tower is 8 to 12 % of tower volume against
1 to 6 % in case of packed tower. So the packed tower offers a smaller liquid residence
time and is more suitable for processing heat sensitive liquids.

5. Corrosive System: For corrosive system, packed tower with plastic packings like
polypropylene packings, glass fibres reinforced plastic packings, etc. is more economical
than tray tower made from special metal alloys.
6. Foaming liquids: It is difficult to process a foaming liquid in a tray tower
since bubbling aggravates the problem of foaming and flooding. The
problem is less severe in a packed tower.

7. Suspended solids: The packings are more prone to deposition and choking
if the liquid has suspended solids in it. A tray tower can handle a dirty liquid Or a
slurry with relative ease . Also, it can be cleaned easily.

8. Side products: If the side products are to be drawn from the distillation
column, like the distillation column of refinery, tray tower is preferred.
Tray Tower :

Tray :

A tray has two major functions:

1. It allows the gas to flow through the holes or passages; the gas vigorously bubbles
through the liquid to from a gas-liquid dispersion. The tray holds the dispersion on it.

2. The trays separate the column in to a number of compartments each of which


constitutes a stage. Mass transfer between phases occurs on a tray. The performance of
a column depends upon the performance of the trays.

Types of Trays :

1. Bubble cap plate

2. Valve plate

3. Sieve plate
Bubble Cap Tray Valve Tray

Sieve Tray
Selection of Tray Type:
Definition of tray areas :
Total tower cross-section area (AT): The empty tower inside cross-sectional area
without trays or downspouts/downcomer.

Net area (AN) (also called free area): The total tower cross-sectional area (AT)
minus the area at the top of the down comer (ADT). The net area symbolizes the
smallest area available for vapor flow in the inter-tray spacing.

Bubbling area or active area (AA): The total tower cross-sectional area minus sum
of the downcomer top area (ADT) and downcomer seal area (ADB) and any other non
perforated areas on the tray. The bubbling area represents the area available for
vapor flow just above the tray floor.

Hole area (Ah): The total area of the perforations on the tray. The hole area is the
smallest area available for vapor/gas passage.
Typical cross-flow plate (sieve)
Dumping
Tower Diameter and Pressure Drop (For sieve tray):

The required diameter of the column for the given flow rates of the gas and the liquid phases
is determined from flooding considerations.

As the gas velocity in a column is gradually increased, a limiting velocity is attained above
which entrainment is high enough to cause accumulation of liquid on the trays leading to
flooding.

This velocity corresponds to the theoretical maximum capacity of the column.

Methods of Calculating Flooding Velocity:

Fairs Method:
This method is based on Souders-Brown equation,
0.2 O .5
L G
vF C f
20 G
Where, V = vapor density, kg/m3
L= liquid density, kg/m3
= liquid surface tension, mN/m (dyn/cm)
0.2 O .5
L G
vF C f
0 .02 G

when, = liquid surface tension, N/m


In above equation Cf is Souders-Brown flooding constant.
But in reality its not constant, as it depends upon tray spacing and liquid load.

Cf can be obtained from a chart given as a function of a flow parameter, FLV for
different values of the plate spacing.

L V
FLV
V L
Where,
L = liquid flow rate, kg/s
V = vapor flow rate, kg/s
V = vapor density, kg/m3
L= liquid density, kg/m3
This figure of flooding velocity, gives flooding velocity with 10% error
subject to following Restrictions:

1. Hole size less than 13 mm. Entrainment may be greater with larger
hole sizes.

2. Weir height less than 15 per cent of the plate spacing.

3. Non-foaming systems.

4. Value of Cf obtained is valid only if Ah/AA 0.1

For other ratios apply the following corrections by multiplying


obtained
value of Cf by correction factors

Ah/AA Correction Factor


0.08 0.9
0.06 0.8
Lygeros and Magoulas have given and algebraic equation for calculating Cf,


C f 0.03445 5.42110 3 S 0.755 exp 1.463FLV0.842

Where, S = tray spacing inches


Checking of Liquid Entrainment:

As a rough guide, the % liquid entrainment should be less than 10%.

Or in other words fractional liquid entrainment should be less than 0.1.

kg of liquid entrained Mole of liquid entrained



kg of gross liquid flow Moles of gross liquid flow

Where, = Fraction liquid entrainment

Value of as a function of liquid-vapor factor (FLV) with different %


of flood as is given in the figure shown.

From this figure value of obtained at calculated percent flood.

Actual vapor vel ocity based on net area


% of flood 100
Flooding velocity
vn
100
vf
Checking for weeping:

At a very low value of vapor velocity liquid rain down through the perforations,
this phenomena is known as weeping.

Weeping tendency increases with


i. Larger fractional hole area
ii. Larger liquid rate
iii. Larger weir height
iv. Lower surface tension of the liquid
v. Decreasing plate thickness
vi. Closer hole spacing or pitch.

Minimum vapor velocity required to avoid the weeping is given by,

K 0.9(25.4 d h )
vh min
v
Where, d= hole diameter, mm,

v = vapor density, kg/m3 (maximum value of vapor density)

K = constant, which is function of depth of clear liquid on the plate, which can be
obtained from figure given
Depth of Clear Liquid = Height of weir + Height of liquid crest over the weir
= hw + hwc

The height of the liquid crest over the weir can be estimated using the
Francis weir formula,

Where, lw = weir length, m,


hw c = weir crest, mm liquid,
Lw = min. liquid flow-rate, kg/s. which can be taken as 70 to
80 % of max. liq. Flow rate
Total Pressure Drop Sieve Tray Tower:

Total pressure drop in sieve tray tower pT is given by,

pT = (Pressure drop per Tray x No. of Trays) + Pressure drop in inlet nozzle +
Pressure drop in outlet nozzle

But, major pressure drop in vapor is provided by trays, therefore,

pT = (Pressure drop per Tray x No. of Trays)

pT = N x pt

Where, N = Total Number of sieve trays of tower


pt = Tray pressure drop , Pa
Again,
pt = 9.81 x 10-3 ht L

ht = hd + (hw + hwc) + hr
Dry plate pressure drop (hd):

Dry plate pressure drop occurs due to friction within dry short holes. can
be calculated using following expression derived for flow through orifices,

2
vh v
h d 51
Co L
Where, hd = Dry plate pressure drop, mm LC

vh = Velocity of gas through the holes, m/s


Volumetric flow rate of gas, m 3 / s QV
=
Total hole area, m 2 Ah

Co = Orifice coefficient which is a function of ratio of


plate thickness to hole diameter and % perforated
area.
Residual gas pressure head (hr):

The residual pressure drop results mainly from the surface tension as the gas
releases from a perforation.

The following simple equation can be used to estimate hr with reasonable


accuracy
12.5 103
hr
L

Where,
hr = Residual pressure drop, mm LC
L = Density of liquid, kg/m3
lw
Weir Design: To decide weir height and weir length
hw
The height of weir decides the height of liquid over the tray.

Weirs are straight and rectangular plates.

A high weir provides higher plate efficiency but at the expense of pressure drop.

For a distillation column:

Operating pressure Weir Height

At and above atm. Pressure. 40 to 90 mm (while 40 to 50 mm is common)

Vacuum Operation 6 mm to 12 mm

Weir length fixes area of segmental down comer. Weir length is normally kept in
between 0.6 to 0.85 times column diameter.

For the first trial calculations, weir length can be taken as 0.77 Di and equivalent
down comer area is 12 %.
Decrease in weir length increases the net area of tray and decreases the tower
diameter, but it decreases the down comer area, increases the pressure drop in down
comer and also decreases the volume of down comer. It also elevates the liquid level
in down comer. Increase in weir length increases the tower diameter. Hence,
balanced weir length and weir height are required.

Weir length lw Down comer area A d


100
ID of tower Di Column area A c
0.600 5.25

0.650 6.80

0.700 8.80

0.705 9.00

0.715 9.50

0.727 10.00

0.745 11.00

0.770 12.00

0.780 13.00
Ad
lw

Section of a sieve tray with down comer

From above fig. fractional down comer area (Ad/Ac) can be


calculated as,

Ad sin

Ac 2
Design of Down comer:
There are two functions of a down comer,

a) It provides the passage for the flow of liquid.

b) Foamy or frothy liquid enters into down comer. Hence, down comer
also acts as a vapor-liquid separator. To facilitate the vapor-liquid
disengagement, certain minimum residence time (at least 3 seconds) is
required in the down comer.

Types of down comer:

Straight segmental Inclined Segmental Circular or Pipes


down comer down comer down comer
The Packed Tower:
A packed tower is a continuous contact equipment widely used for gas absorption,
distillation and liquid-liquid extraction.

It consists of a cylindrical shell filled with a suitable packing material to provide large
interfacial area contact between the phases.

Classification of Packings:

i. Random or dumped packings

ii. Structured packings

iii. Grid packings


(a) Raschig rings

(b) Pall rings

(c) Berl saddle ceramic

(d) Intalox saddle ceramic

(e) Metal Hypac

(f) Ceramic, super Intalox


Grid
Characteristics of Tower Packings:

i. A large surface area: Interfacial area of contact between the gas and liquid is created
in a packed bed by spreading of the liquid on the surface of the packing. Smaller
packings offer a larger area per unit packed volume, but the pressure drop per unit
bed height becomes more.

ii. Uniform flow of the gas and the liquid: The packed bed must have a uniform voidage
so that a uniform flow of the gas and of the liquid occurs. The shape of the packing
should be such that no stagnant pocket of liquid is created in the bed. A stagnant
liquid pool is not effective for mass transfer.

iii. Void volume: A packed bed should have a high fractional voidage so as to keep the
pressure drop low.

iv. Mechanical strength: The packing material should have sufficient mechanical strength
so that it does not break or deform during filling or during operation under the weight
of the bed.

v. Fouling resistance: Fouling or deposition of solid or sediment within the bed is


detrimental to good tower operation. Bigger packings are less susceptible to fouling.
Also, the packings should not trap fine solid particles that may be present in the liquid.
Minimum Wetting Rate:

It is the liquid throughput below which the film on the packing surface breaks up reducing
the wetted area.

A liquid rate below MWR is too small to wet all the packing surface. The effective interfacial
area of the gas-liquid contact decreases and the efficiency of mass transfer decreases as a
result.

Schmidt has given the correlation for MWR as follows,

2 1
2
6 L
3
9 g
u sL 7.7 10 4 L
m3/m2.h
a
L g p
Bed Pressure Drop and The Phenomena of Loading and Flooding in Packed Tower
Determination of Tower Diameter in Packed Tower

For packed tower, diameter of tower is determined based on flooding velocity. Actual
velocity of gas through packed tower is kept about 60 to 80 % of flooding velocity.

Flooding velocity is determined by using Eckerts chart ( Generalized pressure drop


correlation) and proceeds as follows:

i. From the total liquid and gas flow rates the abscissa (FLV) is evaluated.

L V
FLV
V L
ii. The value of the ordinate K is obtained from the flooding curve and the mass flow
rate of the gas G at flooding is calculated.

iii. The operating gas rate is normally taken as 60 to 80 % of flooding velocity to guard
against inherent errors in the flooding curves and also to keep some flexibility in the
design to take care of any sudden surge in gas flow rate.

The relation between K and FLV is given in Eckerts Chart on next slide
K = is given by... (next slide)
2
GF FP L0.2
K
G L g
Where,
GF = Mass velocity of gas at flooding, kg/m2.s
K = Function of velocity of gas through tower
G , L = Density of gas and liquid, respectively, kg/m3
FP = Packing Factor, m-1
= Ratio of density of water to density of liquid
L = Viscosity of liquid, cP

Alternatively an algebraic correlation for the Eckerts flooding curve has been given by
Piche as,

log10 K 0.296logFLV 1.08 log FLV 1.668


2
Design of Packed Bed (Determination of Packed height for gas absorption column):

Height of packing required for a given separation is determined by,

Z HOG NOG (1)

OR

Z HOL NOL (2)


Where,
Z = Height of packed bed

HOG = Height of overall gas phase transfer units, m

NOG = Number of overall gas phase transfer units

HOL = Height of overall liquid phase transfer units, m

NOL = Number of overall liquid phase transfer units

If overall resistance to mass transfer is controlled by gas film then equation (1) is used to find the packing
height Z.

If overall resistance to mass transfer is controlled by liquid film then equation (2) is used to find the packing
height Z.
FOR CONCENTRATED GASES:
As we know for this case, the height of packed is determined by using,

Where,

Above equation (a) can be simplified as,

Where,
For dilute concentrations ( less than 10%):

y1
GM dy
Z
K G aP y2 y ye

On comparing above equation with equation (1)

Gm
H OG
K G aP

y1
dy
N OG
y2
y ye
Where,
Gm = Molar flow rate of gas per unit cross sectional area,
kmol/m2.s
KG = Overall gas phase mass transfer coefficient,
kmol/(atm.m2.s)
a = Interfacial area per unit volume, m2/m3
P = Operating pressure, atm

In the special case, if equilibrium curve and operating line, both can be assumed as
straight lines and the solvent feed essentially solute free, NOG can be calculated by
equation,
1 mGm y1 Gm
N OG ln 1 m
mGm Lm y2 Lm
1
Lm
Where,
m = Slope of equilibrium line
Gm/Lm = Slope of operating line
When the operating and equilibrium lines are straight, and they can usually be
considered to be so for dilute systems, the number of transfer units is given by:

y1 y2
N OG
ylm
where ylm is the log mean driving force, given by:

Where,
Similarly,
x1
LM dx
Z x xe x
K L aCT 2

LM
Thus,
H OL
K L aCT and

x1
dx
N OL
x x
x2 e

Where,
Lm = Molar flow rate of liquid per unit cross sectional area,
kmol/m2.s
KL = Overall liquid phase mass transfer coefficient,
kmol/(atm.m2.s)
a = Interfacial area per unit volume, m2/m3
CT = Total molar concentration, kmol/m3
Analytical Determination of Number of Overall Transfer Units:

If the gas and the liquid stream are dilute and the Henrys law is applicable,

y1 mx2
ln (1 S ) S
y2 mx2
N OG
1 S
Where,
S 1 mG and A absorption factor
A L
Algebraic Determination of the Number of Ideal Stages (Kremser Euqation):

Y mX o 1 1
log N 1 1
Y1 mX o A A
N
log A

Where,
Y and X composition of gas and liquid in molar ratio, respectively.
A Absorption factor
HETP:
The height equivalent to theoretical plate (HETP) is the height of packing that gives the
same separation as an equilibrium stage.

For the distillation in packed tower, height of packed bed Z, required for the desired
separation, is determined by following equation,

Z = Nt x HETP

Where, Nt = Number of theoretical stages required for the desired separtion.

Also see, page no. 453 of the Book Introduction to Process Engineerin
And Design by Bhatt and Thakore.

Relationship between HETP and HOG:


1
ln1 A
HETP H OG
1 1
A

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