Distillation

Distillation
By
Hanapi Bin Mat, Ph.D

Department of Chemical Engineering,
Universiti Teknologi Malaysia,
Skudai, Johor.
Section : 04
Sunday : 09.00 - 10.00 [N02/1-7]
Thursday : 02.00 - 04.00 [N02/1-12]
1
1. Introduction
• Separation of different components in a liquid solution
• Involved producing a vapour from a

liquid by heating the liquid in a vessel
• eg. Ethanol-water:
vapour phase = higher conc. of ethanol
liquid phase = higher conc. of water
• 2 methods of distillation:
 Rectification/fractional/distillation with reflux
– part of the vapour is condensed & returned as
liquid back to the vessel
 All of the vapour is removed or is condensed
as product
2
3
Types of distillation:
• Simple
• Fractional
• Steam
 Immiscible solvent
 Azeotropic
• Extractive
 Vacuum
 Molecular
Distillation tower at an oil refinery.  Entrainer sublimation
4
2. Vapor-liquid equilibrium relations
2.1 Raoult’s
law • Vapor & liquid in intimate contact for a long time,
equilibrium is attained
• Ideal solution (substances very similar to each other)
p A = P Ax A or yA =(pA/P)=(PA/P)xA
where
pA = Partial pressure of component A in the vapor
PA = Vapor pressure of pure A

P = Total pressure
xA = Mole fraction of A in the liquid
yA = mole fraction of A in the gas
5
Example 11.1-1 Use of Raoult’s Law for Boiling-Point Diagram
Calculate the vapor and liquid composition in equilibrium at 95 oC for

benzene-toluene using the vapor pressure from Table 11.1-1 at 101.32 kPa
At 95 o C from Table 11.1 - 1 for Benzene,

PA  155.7 kPa
PB  63.3 kPa
PA x A  PB (1  x A )  P
155.7( x A )  63.3(1  x A )  101.32 kPa
 x A  0.411, x B  1  x A  1  0.411  0.589
PA x A 155.7(0.411)
yA    0.632
P 101.32
6
7
2.2 Boiling-point diagrams and x-y plots
Vapor-liquid equilibrium for A-B mixture e.g. benzene(A)-toluene (B)
 Heat a mixture of benzene-toluene at xA1 = 0.318 (boil at 98oC), first

vapor in equilibrium is yA1 = 0.532
 Distance between equilibrium & 45o line = difference between xA & yA (
Grater difference, easier separation)
8
2.3 VLE diagrams
 Non-ideal systems which will present more difficult separation
 An azeotrope is a liquid mixture which when vaporized, produces the same

composition as the liquid.
9
2.4 Relative volatility of vapor-
liquid system
Relative volatility,  - numerical measure of ease of separation
AB - relative volatility of component A with respect to component B
yA
x y A /x A
AB  yA     
B 1 y /1 x 
xB  A   A 
where

yA = mole fraction of A in the vapor phase
xA = mole fraction of A in the liquid which is in equilibrium with y A phase
10
For an ideal system (obeys Raoult’s law):
x A
yA 
1  1x A
where

PA vapour pressure of pure A

AB  
PB vapour pressure of pure B

when   1 , separation is possible
11
Example 11.3-1 Relative Volatility for Benzene-Toluene System
Using the data from Table 11.1-1, calculate the relative volatility for the
benzene-toluene system at 85oC and 105oC
At 85o C, for a system following Raoult's Law,

P 116.9
 A   2.54
PB 46.0
Similarly at 105 o C,
204.2
  2.38
86.0
The variation in  is about 7%
12
3. Equilibrium Stages - Single-stage
equilibrium
contactor
Binary distillation - components A & B
yA1 yA2
xA0 xA1
Constant molal overflow: V1 = V 2

L0 = L1
Total material balance: L0 + V2 = L1 + V1

Balance on A: L0xA0 + V2yA2 = L1xA1 + V1yA1
Unknown : x1 & y1 – solve simultaneously (graphically) between equilibrium line

& overall material balance
13
Example 11.2-1 Equilibrium Contact of Vapor-Liquid Mixture
A vapor at the dew point and 101.32 kPa containing a mole fraction of
0.40 benzene (A) and 0.6 toluene (B) and 100 kg mol total is contacted
with 110 kg mol of a liquid at the boiling point containing a mole fraction
of 0.30 benzene and 0.70 toluene. The two streams are contacted in a
single stage and the outlet streams leave in equilibrium with each other.
Assume constant molal overflow. Calculate the amounts and compositions
of the exit streams.
14
=100 kmol
Example 11.2-1
yA1 yA2 =0.4
=110 kmol xA1

xA0 =0.3
Constant molal overflow: V1 = V2= 100 kmol
L0 = L1 = 110 kmol
Balance on A: L0xA0 + V2yA2 = L1xA1 + V1yA1
110(0.3) + 100(0.4) = 110xA1 + 100yA1

lets xA1 = 0.2, yA1 = 0.51
lets xA1 = 0.4, yA1 = 0.29
lets xA1 = 0.3, yA1 = 0.4

At intersection, xA1 = 0.25, yA1 = 0.455
15
4. Distillation methods
Distillation has two main methods in practice.
1. Production of vapor by boiling the liquid mixture to be separated in a

single stage and recovering and condensing the vapors. No liquid
is allowed to return to the single-stage still to contact the rising
vapors.
2. Returning of a portion of the condensate to the still. The vapors

rise through a series of stages or trays, and part of the condensate
flows downward through the series of stages or trays counter-
currently to the vapors (“fractional distillation, distillation with reflux,
or rectification”).
16
4. Distillation methods
Simple
distillation
Vapor produced on boiling of liquid
mixture may simply taken of and
condensed without return to the
still.
Distillati
on Does not involved fractionation
 Flash or equilibrium distillation
 Differential distillation
 Steam distillation
Fractional
distillation
Distillation with reflux or
rectification
Batch vs. continuous
17
(a) Equilibrium or flash
distillation
• Single stage binary distillation

• Liquid mixture partially vaporized
• Vapor allowed to come to equilibrium with liquid
• Vapor & liquid then separated
Balance on A:
FxF = Lx + Vy or FxF = (F-V)x + Vy
Unknown : x & y – solve simultaneously (graphically) between equilibrium line

& overall material balance similar to e.g. 11.2-1
18
(b) Simple batch or differential
distillation
V, y • Liquid mixture charged to a still (heated kettle)
• Slowly boiled & vaporized part of the liquid
• Vapor withdrawn rapidly to condenser
L, x • First portion of vapor = richest in component A
• Vaporized product gets learner in component A
L1 = Original moles charge L1 x dx

ln 
L 2 x y  x
1
x1 = Original composition
Graphical solution:
L2 = Moles left in the still L1
Area under the curve 1/(y-x) vs x plot = ln L2
x2 = Final composition of liquid
unknown: x2 Average composition of total material distilled, y av:
L1x1 = L2x2 + (L1-L2)yav 19
Example 11.3-2 Simple Differential Distillation
A mixture of 100 mol contaning 50 mol % n-pentane and 50 mol % n-heptane is

distilled under differential conditions at 101.3 kPa until 40 mol is distilled. What
is the average composition of the total vapor distilled and the composition of the
liquid left? The equilibrium data are as follows, where x and y are mole fractions
of n-pentane.
20
Example 11.3-
2
Equilibrium data:
L1 = 100 mol
x 1.0 0.867 0.594 0.398 0.254 0.145 0.059
x1 = 0.5 mol /mol 0
y 1.0 0.984 0.925 0.836 0.701 0.521 0.271
V = 40 mol Total
0 balance : L1 = V + L2
x2 = ? , yav = ? 100 = 40 + L 2
L2 = 60 mol
L1 x dx
ln 
L 2 x y  x
1
ln 100  x0.5 ydx

 x  0.51
60 2
L1x1 = L2x2 + (L1-L2)yav

By trial & error, x2 = 0.277
100(0.5) = 60(0.277)+ (100-60)yav
yav = 0.835
21
(c) Simple steam
distillation
Note that by steam distillation, as long as water is present,

the high-boiling component B vaporizes at a temperature
well below its normal boiling point without using a vacuum.
The A (water) and B are usually condensed in condenser and
the resulting two immiscible liquid phases separated.
Disadvantage: large amounts of heat must be used to
simultaneously evaporate the water with high-boiling
22
compound.
(c) Simple steam
distillation
When the sum of the separate vapor pressures equals the total pressure,
the mixture boils and
PA  PB  P
Where
PA is vapor pressure of pure water A
PB is vapor pressure of pure B
Then the vapor composition is

P P
yA  A yB  B
P P
The ratio moles of B distilled to moles of A distilled is
nB PB

n A PA
23
Ex 4.6 A mixture contains 100 kg of H2O and 100 kg of
ethyaniline (mol wt = 121.1 kg/kg mol), which is immiscible with
water. A very slight amount of nonvolatile impurity is dissolved in
the organic. To purify the ethyaniline it is steam-distilled by
bubbling saturated steam into the mixture at a total pressure of
101.32 kPa (1 atm). Determine the boiling point of the mixture
and the composition of the vapor. The vapor pressure of each of
the pure compounds is as follows (T1):
Temperature PA(water) PB(ethylaniline)

K ºC (mm Hg) (mm Hg)
353.8 80.6 48.5 1.33

369.2 96.0 87.7 2.67
372.3 99.15 98.3 3.04
386.4 113.2 163.3 5.33
24
PA  PB  P Solution:
Temperature PA PB P=PA+PB
K ºC (water) (ethylaniline) (kPa)
(kPa) (kPa)
353.8 80.6 48.5 1.33 49.83

369.2 96.0 87.7 2.67 90.37
372.3 99.15 98.3 3.04 101.34
386.4 113.2 163.3 5.33 169.23
The boiling temperature = 99.15ºC since total pressure in this temperature

is equal to atmospheric pressure.
The vapor composition are:
P 98.3kPa PB 3.04
yA  A   0.97 yB    0.03
P 101.32kPa P 101.32
25
Distillation calculations
McCabe -Thiele Method
 Equilibrium line
 Operating line - enriching
 operating line - Stripping
 Feed conditions
 Feed location  Number of
 Total reflux stages
 Minimum reflux  Efficiency
 Operating reflux
 Stripping - column distillation
 Flooding
 Enriching - column distillation velocity
Binary system  Rectification with direct steam injection  Tower
 Rectification tower with side stream

diameter
Tray and packed tower efficiency
 Flooding velocity and diameter
of tray towers
Enthalpy-Concentration Method
 Enthalpy – concentration data
 Enriching section
 Stripping section
Multicomponents 26
Distillation calculations
Multicomponents Multicomponent distillation

 Introduction
 Equilibrium data
 Boiling point, dew point and flash distillation
 Key components
 Total reflux
 Minimum reflux ratio
 Operating reflux ratio
 Short cut method for number of stages
27
5. Distillation with Reflux and McCabe-Thiele Method
5.1 Introduction to distillation with reflux
Rectification (fractionation) or stage distillation with reflux is

a series of flash-vaporization stages are arranged in a series which the vapor and liquid
products from each stage flow counter-currently to each other.
The liquid in a stage is conducted or flows to the stage below and the vapor from a stage
flow upward to the stage above.
A total material balance: Vn 1  Ln 1  Vn  Ln
A component balance on A: Vn 1 y n 1  Ln 1 x n 1  Vn y n  Ln x n
28
Introduction to distillation with reflux
In a distillation column the stages (referred to as sieve plates or trays) in a distillation tower are
arranged vertically, as shown schematically in figure below.
1. Feed enters the column somewhere in

the middle of the column.
2. Feed is liquid, it flows down to a sieve

tray or stage.
3. Vapor enters the tray and bubbles

through the liquid on this tray as the
entering liquid flows across.
4. The vapor and liquid leaving the tray

are essentially in equilibrium.
5. The vapor continues up to the next tray

or stage, where it is again contacted with
a downflowing liquid.
6. The concentration of the more volatile

component is being increased in the
vapor form each stage going upward and
decreased in the liquid from each stage
going donwards.
29
Introduction to distillation with reflux
In a distillation column the stages (referred to as sieve plates or trays) in a distillation tower are
arranged vertically, as shown schematically in figure below.
7. The final vapor product coming

overhead is condensed in a condenser
and a portion of the liquid product
(distillate) is removed, which contains a
high concentration of A.
8. The remaining liquid from the

condenser is returned (refluxed) as a
liquid to the top tray.
9. The liquid leaving the bottom tray

enters a reboilier, where it partially
vaporized, and the remaining liquid, which
is lean in A or rich in B, is withdrawn as
liquid product.
10. The vapor from the reboiler is sent

back to the bottom stage or trays is much
greater.
30
5.2 McCabe-Thiele method
• Graphical method for determining the number of theoretical stages, N
A mathematical – graphical method for determining the number of theoretical trays

or stages needed for a given separation of a binary mixture of A and B has been
developed by McCabe and Thiele.
The method uses material balances around certain parts of the tower, which give
operating lines and the xy equilibrium curve for the system.
Main assumption
1) Equimolar overflow through the tower between the feed inlet and the top tray and
the feed inlet and bottom tray.
2) Liquid and vapor streams enter a tray, are equilibrated, and leave.
31
A total material balance:
Vn 1  Ln 1  Vn  Ln
A component A balance:
Vn 1 y n 1  Ln 1 x n 1  Vn y n  Ln x n
Where
Vn+1 is mol/h of vapor from tray n+1
Ln is mol/h liquid from tray n
yn+1 is mole fraction of A in Vn+1 and so on.
32
(a) Equation for enriching section
F  D W (1)
Fx F  Dx D  Wx w (2)
Where
F is the entering feed (mol/h)
D is the distillate (mol/h)
W is the bottoms (mol/h)
33
Material balance over dashed-line section: Vn 1  Ln  D (3)
A balance on component A: Vn 1 yn 1  Ln xn  DxD (4)
34
Solving for yn+1, the enriching-section operating line is
Ln Dx
yn 1  xn  D (5)
Vn 1 Vn 1
Since Vn 1  Ln  D, Ln / Vn 1  R /( R  1)and equation becomes
R x
y n 1  xn  D (6)
R 1 R 1
where R  Ln / D = reflux ratio = constant.

The eqn. (1) is a straight line on a plot of vapor composition versus liquid
composition.
35
The slope is Ln / Vn 1 or R /( R  1) . It intersects the y=x line (45º diagonal
line) at x  x D . The intercept of the operating line at x = 0 is y  xD /( R  1) .
The theoretical stages are determined by starting at xD and stepping off the first
plate to x1. Then y2 is the composition of the vapor passing the liquid x1.
In a similar manner, the other theoretical trays are stepped off down the tower in
the enriching section to the feed tray.
36
(b) Equation for stripping section
Material balance over dashed-line section: Vm 1  Lm  W (7)
A component A balance: Vm 1 ym 1  Lm xm  Wxw (8)
37
Solving for ym+1, the stripping-section operating line is
Lm Wx
ym 1  xm  W (9)
Vm1 Vm 1
Again, since equimolal flow is assumed, Lm  LN = constant and

Vm 1  VN
= constant,
L  Veqn. (2) is a straight line when plotted as y versus x,
m m 1
with a slope of . yIt 
intersects
Wx / Vthe y = x line at x = xw.
W m 1
The intercept at x = 0 is .
38
The theoretical stages for the stripping section are determined by starting at
xW, going up to yW, and then across to the operating line, etc.
39
(c) Effect of feed conditions
The condition of feed stream is represented by the quantity q, which is the mole
fraction of liquid in feed.
Lm  Ln  qF (10)
Vn  Vm  (1  q ) F (11)
The enriching and striping operating-line

equations on an xy diagram can be
derived as follows:
Vn y  Ln x  Dx D (12)
Vm y  Lm x  Wx w (13)
Where the y and x values are the point of

intersection of the two operating lines.
Subtracting eqn.(12) from eqn.(13),
(Vm  Vn ) y  ( Lm  Ln ) x  ( Dx D  Wx w ) (14)
40
Substituting eqn.(2), (10), and (11) into eqn.(14) and rearranging,
q x
y x F
q 1 q 1
(15)
c pL (Tb  TF )
q  1

Cold-liquid feed Superheated vapor
where
CpL, CpV = specific heats of liquid and vapor, respectively
TF = temperature of feed
Tb, Td = bubble point and dew point of feed respectively
λ = heat of vaporization
41
L V L V L V
F F F
dew point
L bubble point
q=0
liquid feed q=1 vapour feed
L V L V L V
F F F
subcooled superheated partially vaporized

liquid feed
q>1 vapour feed
q<0 feed
0<q<1
42
q = moles of liquid flow in the stripping section L L
that result from the introduction of each mole of q
F
feed
q = 1 (liquid at its boiling point)
q = 0 (saturated vapour) q>1
q=1
x
q  1 (cold liquid feed)
y=
q  0 (superheated vapour) 0<q<1
0  q  1 (mixture of liquid & vapour)
Feed a mixture of liquid & vapour, q q=0
= fraction that is liquid xF
 
q  xF

y  x 
q1  q1


q<0

43
(d) Location of the feed tray in a tower and number of trays
From eqn.(15), the q-line equation and is the locus of the intersection of the two
operating lines. Setting y = x in eqn(15), the intersection of the q-line equation
with the 45º line is y=x=xF, where xF is the overall composition of the feed.
In given below the figure, the q line is plotted for various feed conditions. The
slope of the q line is q/(q-1).
q = 0 (saturated vapor)
q = 1 (saturated liquid)
q > 1(subcooled liquid)
q < 0 (superheated vapor)
0 < q < 1 (mix of liquid and
vapor)
44
(e) Number of stages and trays
1st point
2nd point
3rd point
n = 7 = Number of tray + reboiler
Number of tray = 6 45
Slope = R/(R+1)
Slope = q/(1-q)
Slope = L/ V
46
(f) Reflux Ratio
Total Reflux Ratio
One limiting values of reflux ratio is that of total reflux or R = ∞. Since R

= Ln/D and, by eqn.(16).
Vn 1  Ln  D (16)
Then Ln is very large, as is the vapor flow Vn. This means that the slope
R/(R+1) of the enriching operating line becomes 1.0 and the operating
lines of both sections of the column coincide with the 45º diagonal line,
as shown in Fig below.
Minimum number of trays can be obtained by returning all the overhead

condensed vapor V1 from the top of the tower back to the tower as
reflux, i.e., total reflux. Also, the liquid in the bottoms is reboiled.
47
 x 1  xw 
Minimum number of theoretical steps Nm log D 
Nm   1  xD xw  (17)
when a total condenser is used (α is constant).
log  av
For small variations in α,  av   1 w 
1/ 2
(18)
where α1 is the relative volatility of the overhead vapor
αw is the relative volatility of the bottoms liquid.
48
48
Total reflux, R = ∞
R= ∞ then R/(R+1)=1
• operating lines coincide with 45o line

• minimum number of stages, Nmin
• infinite sizes of condenser,
reboiler
& tower diameter
• or using Fenske equation (total condenser)

xD 1 x W 
log

x W 
1 x D
Nmin 
log av
av = average value of relative volatility

(1W)volatility
1==relative ½
of the overhead vapour
W= relative volatility of the bottom liquid 49

49
Total reflux, R = ∞
R= ∞ then R/(R+1)=1
• operating lines coincide with 45o line

• minimum number of stages, Nmin
• infinite sizes of condenser,
reboiler
& tower diameter
• or using Fenske equation (total condenser)

xD 1 x W 
log

x W 
1 x D
Nmin 
log av
av = average value of relative volatility

(1W)volatility
1==relative ½
of the overhead vapour
W= relative volatility of the bottom liquid 50

Minimum Reflux Ratio
The minimum reflux ratio (Rm) will require an infinite number of trays for the given
separation desired of xD and xW.
If R is decreased, the slope of the enriching operating line R/(R+1) is
decreased, and the intersection of this line and the stripping line with the q line
moves farther from the 45º line and closer to the equilibrium line.
Two operating lines touch the

equilibrium line (“pinch point”) at y’
and x’ (number of steps required
becomes infinite).
The line passes through the points x’,
y’ and xD (y=xD):
Rm x  y
 D (19)
Rm 1 xD  x
51
x
Enriching op. line: y  R x D
R 1 R 1
If R decreases, then
Both the rectifying, stripping and feed line

eventually will intersect at the equilibrium line.
xF
xW xF xD
y-intercept at Rmin:
xD
 y intercept
Rmin 1
Resulting in an infinite number of plates

52
• or when equilibrium line has an
• minimum vapor flow inflection, operating line tangent to
the equilibrium line
• minimum condenser & reboiler
• Rmin at pinch point (x’,y’)
• Enriching op. line: Slope at Rmin: Rmin x D  y


x Rmin 1 x D  x 
y  R x D
R 1 R 1

53
Enriching op. line:
x
y  R x D
R 1 R 1
If R decreases, then
Both the rectifying, stripping and feed line xF

eventually will intersect at the equilibrium line.
xW xF xD
y-intercept at Rmin:
xD
 y intercept
Rmin 1

Resulting in an infinite number of plates 54
Operating and optimum reflux ratio
Total reflux = number of plates is a minimum, but the tower diameter is infinite.
This corresponds to an infinite cost of tower and steam and cooling water. This
is the limit in the tower operation.
Minimum reflux = number of trays is infinite, which again gives an infinite cost.
These are the two limits in operation of the tower.

Actual operating reflux ratio to use is in between these two limits. The optimum
reflux ratio to use for lowest total cost per year is between the minimum R m and
total reflux (1.2Rm to 1.5Rm).
55
Ex 4.7 A continuous fractioning column is to be designed to separate
30,000 kg/h of a mixture of 40 percent benzene and 60 percent toluene
into an overhead product containing 97 percent benzene and a bottom
product containing 98 percent toluene. These percentages are by weight.
A reflux ratio of 3.5 mol to 1 mol of product is to be used. The molal latent
heats of benzene and toluene are 7,360 and 7,960 cal/g mol,
respectively. Benzene and toluene from a nearly ideal system with a
relative volatility of about 2.5. The feed has a boiling point of 95ºC at a
pressure of 1 atm.
a) Calculate the moles of overhead product and bottom product per hour.
b) Determine the number of ideal plates and the position of the feed plate
(i) If the feed is liquid and at its boiling point;

(ii) If the feed is liquid and at 20ºC (specific heat 0.44 cal/g.ºC);
(iii) If the feed is a mixture of two-thirds vapor and one-third liquid.
56
Solution (a)
40 97 2
78 xD  78  0.974 78
xF   0.440 xB   0.0235
40 60 97 3 2 98
  
78 92 78 92 78 92
100
The average molecular weight of 40  85.8
the feed
60 is

78 92
 vaporization
The average of heat 0.44(7,360)  0.is
56(7,960)  7,696 cal / gmol
The feed rate F is 30,000/85.8 = 350 kg mol/h. By an overall benzene

balance, using Eq. below
 0.440  0.0235 
D  350   153.4kgmol / h
 0.974  0.0235 
B  350  153.4  196.6kgmol / h
57
Solution (b) (i),
We determine the number of ideal plates and position of the feed plate.
1) Plot the equilibrium diagram, erect verticals at xD, xF, and xB.
2) Draw the feed line. Here q=1, and the feed line is vertical.
3) Plot the operating lines. The intercept of the rectifying lie on
the y axis is, xD/(R+1) = 0.974/(3.5+1) = 0.216 (eqn (6)). From the
intersection of the rectifying operating line and the feed line, the stripping
line is drawn.
4) Draw the rectangular steps between the two operating lines
and the equilibrium curve. The stripping line is at the seventh step. By
counting steps it is found that, besides the reboiler, 11 ideal plates are
needed and feed should be introduced on the seventh plate from the top.
58
59
Solution (b) (ii),
The latent heat of vaporization of the feed λ is 7,696/85.8 = 89.7 cal/g.
0.44(95  20)
q  1  1.37
89.7
q x
y x F
q 1 q 1
The slope of the feed line is -1.37/(1-1.37) = 3.70. When steps are drawn
for this case, as shown in Fig. below, it is found that a reboiler and 10
ideal plates are needed and that the feed should be introduced on the
sixth plate.
60
61
Solution (b) (iii),
From the definition of q
it follows that for this
case q = 1/3 and the
slope of the feed line is
-0.5. The solution is
shown in Fig. below. It
calls for a reboiler and
12 plates, with the feed
entering on the
seventh plate.
62
Ex 4.8 What are (a) the minimum reflux ratio and (b) the minimum
number of plates for cases (b)(i), (b)(ii), and (b)(iii) of EX 4.7 if αav
is given as 2.47.
Solution (a)
For minimum reflux ratio use eqn. (18). Here xD = 0.974. The results
are given in Table below.
Case x’ y’ RDm
(b)(i) 0.440 0.658 1.45
(b)(ii) 0.521 0.730 1.17
(b)(iii) 0.300 0.513 2.16
63
Ex 4.8 What are (a) the minimum reflux ratio and (b) the minimum
number of plates for cases (b)(i), (b)(ii), and (b)(iii) of EX 4.7 if αav
is given as 2.47.
Solution (b)
For minimum number of plates, the reflux ratio is infinite, the operating
lines coincide with the diagonal, and there are no differences among
the three cases. Use the αav = 2.47 and equation below we get,
 x 1  xw 
log D 
 1  x x w   0.974  0.976 
Nm  D
 ln  1
log  av  0.024  0.026 
 8.105  1  7
The minimum number of ideal plates is 7 plus a reboiler.
64
Example 11.4-1 Rectification of a Benzene-
Toluene Mixture
A liquid mixture of benzene-toluene is to be distilled in a

fractionating tower at 101.3 kPa pressure. The feed of 100
kg mol/h is liquid and it contains 45 mol % benzene and
55 mol % toluene and enters at 327.6 K. A distillate
containing 95 mol % benzene and 5 mol % toluene and a
bottoms containing 10 mol % benzene and 90 mol %
toluene are to be obtained. The reflux ratio is 4:1. The
average heat capacity of the feed is 159 kJ/kg mol.K and
the average latent heat 32099 kJ/kg mol. Equilibrium data
for this system are given in Table 11.1-1 and in Figure
11.1-1. Calculate the kg moles per hour distillate, kg
moles per hour bottoms and the number of theoretical
trays needed.
65
Example 11.4-1
1. Determine D kmol/h, W kmol/h
Total material balance:

D kmol/h F =100 =D + W
xD = 0.95 D =100 - W
Balance on benzene (A):
F =100 kmol/h
FxF = DxD + WxW
xF = 0.45
100(0.45) = D(0.95) + W(0.1)
TF = 327.6K
Substituting D = 100-W
W kmol/h 45 = (100-W)(0.95) + W(0.1)
xW = 0.1 45 = 95 +(W)(0.95) + W(0.1)
W = 58.8 kmol/h D = 100-58.8 = 41.2 kmol/h

66
Example 11.4-1
L 41.2 kmol/h
xD = 0.95
F =100 kmol/h
1. Plot equilibrium & 45o lines on x-y graph
xF = 0.45
TF = 327.6K 58.8 kmol/hy
xW = 0.1
slope=R/(R+1)
2. Draw enriching
operating line
x
y  R x D
R 1 R 1 1
xD
R 1
xD
67 x
Example 11.4-1
L 41.2 kmol/h
xD = 0.95
F =100 kmol/h
xF = 0.45
TF = 327.6K 58.8 kmol/h
xW = 0.1
2. Draw enriching operating line
x
y  R x D
R 1 R 1
R = 4 = L/D
y  4 x  0.95  0.8x  0.19

4 1 4 1
68
Example 11.4-1
3. Calculate
q
H V  H F  H V  H L   cP (TB  TF )
q 
HV  HL HV  HL
Average heat capacity of feed =159 kJ/kmol.K

Average latent heat 32099 kJ/kmol
32099  (159)(TB  327.6)


q 
32099
From Fig. 11.1-1, at xF = 0.45, TB = 93.5oC
(366.7K)
32099  (159)(366.7  327.6)

q   1.195
32099
69
Example 11.4-1
4. Draw q-
line q-line
q = 1.195
 
 q  xF
y   x
 
q1 
 
q1
y 1.195 x 0.45  6.12x2.31

 1.1951 1.1951
Slope = 6.12 = y/x = (0.45 – y)/

(0.45-x)
Lets x = 0.40
0.45  y
6.12  0.45 - y  0.45 - y 
0.45  x 0.45  0.4 0.05
y = 0.144 5. Draw stripping
operating line
Connect xW (on 45o line) with the point of intersection of
70
the q-line & the enriching operating line
Example 11.4-1
6. Stepping off from 2

1
xD Starting from xD, make steps bet. 3

Feed tray
equilibrium line & enriching line to q- 4
line 5
7. Shift to stripping line after passing q- 6

line
7
8. Feed location = tray on the shift 8
Feed tray = tray 5 from the top
9. Ntheo. stages = number of steps
Ntheo. stages = 8 stages

10. Ntheo. trays = theo. stages - reboiler
Ntheo. trays = 8 – 1= 7 trays plus a reboiler

71
Example 11.4-2 Minimum Reflux Ratio and
Total Reflux in Rectification
For the rectification in Example 11.4-1, where a

benzene-toluene feed is being distilled to give a
distillate composition of xD = 0.95 and a bottoms
composition of xW = 0.10, calculate the following.
(a) Minimum reflux ratio, Rm
(b) Minimum number of theoretical plates at
total reflux.
72
(a) Minimum
Example 11.4-2
Reflux, Rmin
Given R = 4, Rmin = ?
41.2 kmol/h
xD = 0.95 The enriching op. line from xD is drawn
through the intersection of the q-line & the
F =100 kmol/h
equilibrium line to intersect the y-axis
xF = 0.45
58.8 kmol/h
xW = 0.1
Enriching op. line: x
y  R x D
R 1 R 1
y-intercept: xD 0.95
  0.43
R min  1 R  1
min
Rmin = 1.21 73
Example 11.4-2
(b) Total Reflux
At R = ∞, Nmin = ?
Steps are drawn from xD to xW.
41.2 kmol/h
xD = 0.95
F =100
kmol/h
xF = 0.45
58.8 kmol/h
xW = 0.1
Nmin = 5.8 stages or 4.8 trays plus a reboiler

74
McCabe-Thiele method calculation
procedure
1. Calculate the flow rates of D and W using material balances.
2. Plot yA-xA graph with the 45o and equilibrium lines.

Locate points xD, xW and xF
3. Draw enriching operating line

x
y  R x D where R = reflux ratio = L/D
R 1 R 1
4. Calculate q
H V  H F  H V  H L   cP (TB  TF )
q 
H V  HL HV  HL
5. Draw q-line
 
q  xF

y  x 
q1  q1


75
75
6. Draw stripping operating line by connecting x W (on 45o line) with
the point of intersection of the q-line & the enriching operating
line
7. Stepping off from xD between equilibrium line & enriching line to q-
line
8. Shift to stripping line after passing q-line. Feed location = tray on the shift
9. Ntheo. stages = number of steps
10. Ntheo. trays = theoretical stages - reboiler
76
5.3 Distillation column
(a) Stripping
column
• Feed is saturated liquid at boiling point (q=1)
• Added to the top of the column
• Overhead product is not returned back to the tower
Lm Wx W
• Operating line: y x 
Vm  1 m V
m1
• Ntheo. stages - starting from xW(on 45o line) draw a
straight line to the intersection of yD with the q-line
77
Example 11.4-
3
78
(b) Enriching column
• Feed is saturated vapor (q=0)
• Added to the bottom of the column
• Overhead product is refluxed back to the tower
R xD D
• Operating line: y x
R 1 R 1
• N theo. stages - starting from xD(on 45o line) draw a
straight line to the y-intercept, xD/(R+1)
W
F
xF xD
79
(c) Direct steam injection
• Heat provided by open steam injected directly at bottom of tower
• Steam injected as small bubbles into liquid

y  Wx Wx
• Stripping operating line: S W
S
• Draw a straight line from (xW,0) through WxW/(W-S) on
the 45o line
• Use of open steam requires an extra fraction of a stage 80

(d) Side stream
• Stream removed from sections of tower
• Side stream above feed inlet:
LS Ox O  Dx D
intermediate operating line: y  V x 
S 1 V S 1
liquid side stream: Ln = LS+O
VS+1 = Vn+1=V1=Ln+D
• From the intersection of enriching op. line & x O, draw a
straight line to y-intercept of intermediate op. line
81
(e) Partial condenser
• Overhead product = vapour
• Liquid condensate returned to tower as reflux
• One extra theoretical stage for partial condenser (both
liquid & vapour in condenser is in equilibrium)
82
5.4 Tray efficiency
3 types of tray efficiency:
• Overall tray efficiency, Eo
• Murphree tray efficiency, EM
• Point/local tray efficiency, EMP
EO  no. of ideal trays

no. of actual trays
yn - yn  1
EM 
y *n -yn  1
y'n -y'n  1
EMP 
y *n -y'n  1
83
Graphical determination of actual trays given EM:
1 actual tray = triangle ‘abe’ on actual
equil. line
1 ideal tray = triangle ‘acd’ on ideal
equil. line
Eg. EM = 0.6 (60% efficiency)
distance ‘ac’ = 10 cm
distance ‘ab’ = 0.6(10 cm) = 6 cm
Get 4-5 points & draw actual equil.

line thru’ each points
Step off actual trays between
operating & actual equil. lines
Reboiler = 1 stage (bet. ideal equil.
& operating lines
84
Efficiency of random-packed &
structured packed towers
HETP = height of the packed column necessary to give a
separation equal to one theoretical plate

Height of packing, z 1 
ln 


HETP  HOG A 

z  N HETP H OG N OG  / A
1 A
 
where:
 N = number of theoretical stages needed  

m  
NOG = number of tranfer units ln  
L 



HOG = overall height of a transfer unit HETP  HOG V  
m/ L 1


V 
In distillation: Tray tower 
T
HOG  HETP HETP 
E0

where: E0= overall tray efficiency T = tray spacing 85
(a) Efficiency of tray
towers
For distillation
-0.245
E0  0.492 L
where:
Eo= fraction overall ave. tray efficiency
 = relative volatility of the two key components at the ave. tower temp.
L= molar ave. viscosity (cp) of the liquid feed at the ave. temp.
For absorption  2

mM L mM L
  
    
log E0  1.597-0.199log   0.0896 log
L    L 



L 








L 



where:
ML = average molecular weight of liquid

m = slope of equilibrium line (mole fraction)
L= liquid density (Ibm/ft3)
L= molar ave. liquid viscosity (cp) at the ave. temp.

86
(b) Efficiency of random-
packed towers
For random-packing with low-viscosity liquids:
For second-and third-generation packings only (REF:
S2) HETP  0.0180dp
For vacuum service (REF: S3)
 HETP  0.0180dp  0.15

(c) Efficiency of structured packing
towers
For structured packings at low - moderate pressure with low-viscosity liquids:
where HETP  100 a 0.10
HETP = height equal to one theoretical plate (m)


dp = packing diameter (mm) (for 0.3 m < D < 0.6 m, HETP = D)
a = surface area (m2/m3) 87

Example 11.5-1
A liquid feed benzene-toluene is being distilled under the some
conditions as Example 11.4-1. The number of theoretical steps needed is
calculated as 7.6. The feed composition xF = 0.45, xD = 0.95 and xw =
0.10. Do as follows:
(a) Using valve trays, calculate the overall efficiency Eo and the
tower height. Assume a
tray spacing T of 0.6 m.
(b) Using 2-in metal Pall rings, calculate the HETP and the tower
height.
Solution
(c) Using Plexipac No. 2 structured packing, calculate the tower
height.
88
5.5 Flooding velocity and diameter of
tray towers
For maximum allowable vapor velocity for sieve, bubble-cap or valve trays:
 0.2  

For nonfoaming systems: max K 
 L V
20 
 
 V
where
max = Allowable vapor velocity

based active area (ft/s)
 = Surface tension of the liquid (dyn/cm or mN/m)
V , L = Densities of gas and liquid (Ibm/ft3 or kg/m3)
K = Empirical coefficient obtained from Fig. 11.5-3 (ft/s)
Rule of thumb: K multiplied by 0.91 to account for the downspout area of 9% of
the tray
For foaming systems: K multiplied by 0.90
For final design: max multiplied by 0.80 to be 20% below flooding
For organic liquids :  = 20 -25 dyn/cm
For water with =72 dyn/cm, max multiplied by 1.26

89
Fig. 11.5-3 (ft/s)
where
L, V = flow rates (kg/h or Ibm/h)
V , L = densities of gas and liquid (Ibm/ft3 or kg/m3)
K multiplied by 0.91 to account for downspout area
90
Example 11.5-2
A valve tray absorption tower is being used to absorb and recover ethyl
alcohol vapor in air by pure water. The tower operate at 30 oC and a
pressure of 110 kPa abs. The entering gas contains 2.0 mol % ethyl
alcohol in water, and 95 % of the alcohol is recovered in the outlet
water. The inlet pure aqueous flow is 186 kg mol/h and the inlet gas flow
is 211.7 kg mol/h. Calculate the required tower diameter. A tray spacing
of 0.610 m (2.0 ft) will be assumed. Use a factor of 0.95 for possible
foaming.
Solution
91
6. Enthalpy - Concentration Method
Enthalpy-Concentration Method
(Ponchon-Savarit method)
 Enthalpy – concentration data
 Enriching section
 Stripping section
 Complete analysis of fractional
distillation
 Condenser and reboiler duty
 Minimum reflux
 Total reflux
 Operating reflux
 Partial condenser
 Partial vaporized feed
92
6.1 Enthalpy - Concentration Data
Enthalpy-concentration for benzene-toluene
h = xAcpA (T -T0) + (1-xA)cpB(T - T0) + ΔHsol
H = yA[λA+ cpyA (T -T0)] + (1-yA)[λB + cpyB(T - T0)]
λA= λAb at Tref. = To
λB = cpB (TbB -T0) + λBb - cpyB(TbB - T0)]
where T0 = Tref. = Tb.p. of liquid benzene

cpA, cpB= cp of liquid benzene & toluene, ΔHsol = heats of solution = neglected
respectively
λA, λB=latent heat at To
cpyA, cpyB = cp of vapor benzene &
93
toluene, respectively
94
• Calculation shown in eg. 11.6-1 Use of Enthalpy-
Concentration Chart
95
7.2 Fractional Distillation Using Enthalpy-Concentration
Method
Use of Enthalpy-
Concentration Chart
 Using when molal overflow rates are not necessary constant
 The following date needed to construct such a diagram at

constant pressure:
1. Heat capacity of the liquid, c p

2. Heat of solution, ΔH sol
3. Latent heats of vaporization, 
4. Boiling point, Tb
96
Method
Use of Enthalpy-
Concentration Chart
Saturated liquid line in enthalpy h
h  x A c pA (T  To )  (1  x A )c pB (T  To )  H sol
Saturated vapor line in enthalpy H

  
H  y A  A  c pyA (T  To )  (1  y A )  B  c pyB (T  To ) 
where
xA  mole fraction of A
T  boiling point of the mixture
To  references temperature
c pA , c pB  heat capacity of A and B
H sol  heat of solution at To
c pyA , c pyB  vapor heat capacity of A and B
A , B  latent heat at boiling point of pure component A
97
Method
Use of Enthalpy-
Concentration Chart
98
Method
Use of Enthalpy-
Concentration Chart
99
Method
Use of Enthalpy-
Concentration Chart
Overall balance
F V  L (3)
Balance on A
Fx F  Vy D  Lx L (4)
From the equation(3) & (4), we get

V x  xL
 F (5)
L y D  xF
Energy balance
FH F  VH V  Lh L (6)
100
Method
From the equation (3) & (6) we get Use of Enthalpy-

V x  xL H  hL Concentration Chart
 F  F (7)
L yD  xF HV  H F
If we have a system in which q kJ/h or kW(btu/h) is added to the feed stream,

Heat balance :
 q
 H F   F  VH V  Lh L
 F
q
 Total enthalpy of feed : H F 
F
101
Method
102
Method
Overall material balance :
Distillation in Enriching
D V  L Section of Tower
n 1 n
D  V2  L1  V3  L2  .......
The difference between two streams passing each other is constant and
has value of D kg mol/h where D is the distillation flow.
Dx D  Vn 1 y n 1  Ln x n
Dx D  V2 y 2  L1 x1  V3 y 3  L2 x 2  .......
The compositio n of this difference steam is constant at x D
103
Method
Section of Tower
104
Method
Enthalpy balance :
DhD  Vn 1 H n 1  Ln hn Section of Tower
 q 
D hD  c   Vn 1 H n 1  Ln hn
 D
DH '  V3 H 3  L2 h2  .......
The difference in enthalpy between the streams passing each

 q 
other is constant, with the enthalpy of the stream being  hD  c  ,
 D
where q c is the condenser duty in kJ/h or kW(btu/h)
The difference point will be call D ' , having an enthalpy

H  hD  qc /D and composition xD .
Point D' is a common operating point for all values of Vn 1 and Ln

in the enriching section of the distillation tower.
105
Method
Section of Tower
106
Method
Section of Tower
107
Method
Overall material balance : Distillation in Stripping
Lm  W  Vm 1 Section of Tower
W  Lm  Vm 1  LN  VW
This difference between two streams passing each other is constant
at W kg mol/h
For various trays,

W  Lm  Vm 1  Lm 1  Vm  LN  VW  ...
The composition of this difference stream is constant at xw
Enthalpy balance :
Lm H m  q R  WhW  Vm1 H m 1
 q 
W  hW  R   Lm H m  Vm 1 H m 1
 W
WH 'W  Lm H m  Vm1 H m 1
 q 
other is constant with the enthalpy being  hW  R  or H 'W .
 W 108
Method
Distillation in Stripping
Section of Tower
Enthalpy balance :
Lm H m  q R  WhW  Vm 1 H m 1
 q 
W  hW  R   Lm H m  Vm 1 H m 1
 W 
WH 'W  Lm H m  Vm 1 H m 1
 q 
other is constant with the enthalpy being  hW  R  or H 'W .
 W 
109
Method
Analysis of Complete
Fraction Tower
Overall enthalpy :
Reflux ratio ( R)
FH F  q R  DhD  WhW  q C
 qC 
 q   q   hD    H n 1
FH F  W  hW  R   D hD  C  Ln  D
 W   D R 
D H n 1  hn
FH F  WH 'W  DH '
Reflux ratio at the top of the tower:
L H ' H 1
R 
D H 1  hD
110
Method
Analysis of Complete
Fraction Tower
111
Method
Condenser & Reboiler duties
Condenser duty (qC)
qC  V1H1  L D hD
where

L = RD
H1 = Enthalpy of vapour V1
hD = Enthalpy of liquid distillate
Reboiler duty (qR)

Using material balance
qR = DhD + WhW + qC - FhF
where
hW , hF= Enthalpy of liquid bottom product & feed, respectively

112
Method
Minimum Reflux
Rmin occurs when the line ∆RF∆S (or D’FW’) coincides with
the tie line that passes through F
Total Reflux
Nmin is obtained when the operating lines are vertical since R
(or D’) and S (or W’) are at infinity.
Operating Reflux
R = ? Rmin
113
Method
Minimum Reflux
Rmin occurs when the line
∆RF∆S coincides with the tie
line that passes through F
∆Rmin
W
F
D
114
Method
Total Reflux
Nmin is obtained when the
operating lines are vertical
since R and S are at
infinity.
Minimum stages, Nmin
Nmin is obtained
when the operating
W
lines are vertical F
D
since R and S are
at infinity. Nmin = 5.9 stages
115
6.2 Fractional Distillation
yD Using Enthalpy-Concentration
Method
Partial condenser
Distillate product, VD – vapor
with the composition yD
Condensed liquid/reflux, L0, x0

which is in equilibrium with y
∆R
have the composition xo D
V6 V5 V4 V V V V
Partial condenser = 1 stage 3 2 1 D
W L6 L5 L4 L3 L2 L1 L0
F
∆S
116
Method
Partial vaporized feed

F with the composition zF lies
on the tie line LF (composition
= xF) and VF (composition =
yF)
zF
By trial-and-error, locate the
point F so as to satisfy the
inverse lever rule:
VF VF
F
VF FL F W F
 LF LF
LF FVF
117
Analysis of Complete Fraction Tower
Example 11.6-1 Distillation Using Enthalpy-Concentration Plot
A mixture of 50 wt% ethanol and 50% water which is saturated liquid at

the boiling point is to be distilled at 101.3 kPa pressure to give a distillate
containing 85 wt% ethanol and a bottoms containing 3 wt% ethanol. The
feed rate is 453.6 kg/h and a reflux ratio of 1.5 is to be used. Use
equilibrium data and enthalpy data from Appendix A.3. Do as follows:
(a) Calculate the amounts of distillate and bottoms.
(b) Calculate the number of theoretical trays needed using the enthalpy-
concentration plot.
(c) Calculate the condenser and reboiler heat loads.
118
Example 11.6-1
(a)
F  453.6 kg/h
x F  0.5
x D  0.85
xW  0.03
R  L / D  1.5
All equations and graphs plotted use consistent unit of kg/h, kJ/h and wt fraction
Overall Material Balance :

F  453.6  D  W
Ethanol Balance :
0.50(453.6)  0.85 D  0.03W
Solving, D  260 kg/h
W  193.6 kg/h
119
Example 11.6-1
(b)
The enthalpy - concentrat ion plot is constructed in Fig 11.6 - 8 using data from Appendix A.3
An x-y equilibrium plot is also made
L (h  q C / D )  H 1 H ' H 1
R  D 
D H 1  hD H 1  hD
From saturated vapor plot at x D  0.85 in Fig 11.6-8,
H 1  1303kJ/kg
hD  228 kJ/kg
H '1303
1.5 
1303  228
H '  2914 kJ/kg
The operating point D' is plotted at H '  2914 and x D  0.85
Point F is plotted at x F  0.50 on the h line and give hF  286 kJ/kg
120
Example 11.6-1
The oprating point W' for the stripping section is located at intersection of the line through D'F with the
vertical line xW  0.03
The enthalpyW' , H'W  -3133 kJ/kg
As check,
FhF  WH 'W  DH '
453.6(286)  193.6 H 'W 260.0(2914)
H 'W  3243 kJ/kg
(This is close check on the graphical method to determine W' )
121
Example 11.6-1
1. The number of theoretical steps is determined
by starting with V1
2. An equilibrium tie line through V1
establishes L1 on the saturated liquid line
3. An operating line through L1D gives point V2
on the saturated vapor line.
4. A tie line through V2 gives L2
5. This continue till L3 is reaches
6. The equilibrium tie line L3V3 cross line W’FD’
7. For optimum feed plate location, the stripping

operating line should next be used
8. Draw an operating line W’L3, V2 is obtained
9. This is continued as shown in Fig. 11.6-8
10. Hence, 3.9 theoretical trays plus a reboiler are

needed
11. The feed enters on third tray from the top
122
Example 11.6-1
(c)
Solving for condenser load q c ,
qc
H '  hD 
D
qc
2914  228 
260.0
q c  698360 kJ/h  193.99 kW
Solving for reboiler load q R ,

qR
H 'W  hW 
W
qR
 3243  395 
193.6
q R  704317 kJ/h  195.64 kW
123
Example 11.6-2
L 41.2 kmol/h
Given : R = 1.5 Rm = 1.5(1.17) = 1.755
xD = 0.95
F =100 kmol/h
xF = 0.45
TF = 58.8 kmol/h
54.5oC(327.6K) xW = 0.1
hF = xFcpA(TF-T0) + (1-xF)cpB(TF-T0)
= 0.45(138.2)(54.5-80.1) + (1-0.45)167.5(54.5-80.1) = -3938.1 kJ
hD = xDcpA(TD-T0) + (1-xD)cpB(TD-T0)
= 0.95(138.2)(81.1-80.1) + (1-0.95)167.5(81.1-80.1) = 139.67 kJ
hW = xWcpA(TW-T0) + (1-xW)cpB(TW-T0)
= 0.1(138.2)(106-80.1) + (1-0.1)167.5(106-80.1) = 3904.4 kJ

124
Example 11.6-2
1. Plot enthalpy-concentration diagram and x-y diagram on
the same sheet of paper.
Locate points D, W and F at xD, xW and xF, respectively.
hF = xFcpA(TF-T0) + (1-xF)cpB(TF-T0)
where cpA = cp of liquid benzene = 138.2 kJ/kmol.K

cpB = cp of liquid toluene = 167.5 kJ/kmol.K
T0 = Tref. = Tb.p. of liquid benzene = 80.1oC
hF= 0.45(138.2)(327.6-353.1) + (1-0.45)167.5(327.6-353.1) = -3938.1 kJ
125
Example 11.6-2
W
F
D
126
Example 11.6-2
2. Locate rectifying-section difference point, R

 QC 
hD    H1


 D  Δ H
R   R 1
H1  hD Hh 1 D
R
hD+QC/D
ΔR H1
Sat. vapour V1
H1
hDH1
Sat. liquid
hD
127

 QC 
hD 
  H1
 D  Δ H
R   R 1
H1  h D Hh 1 D
 QC 

 hD   H1
 D  Δ H Δ H
R   R 1  1.755  R 1
H1  hD Hh 1cm
1 D
 R =85x 103kJ/kmol ∆R
ΔR H1  1.755 1cm  1.755cm




H1=31x 103kJ/kmol V1
W
F
hW=5x 10 kJ/kmol
3 D
128
Example 11.6-2
3. Locate stripping-section difference point, S
4. Step off trays for rectifying section using R.
5. Step off trays for stripping section using S
6. Theoretical stages = numbers of tie lines
7. Theoretical trays = theoretical stages - reboiler
Theoretical trays = 11.9 – 1 = 10.9 trays
8. Feed tray = tie line that crosses the line Δ R FΔS
Feed trays = tray no. 7 from the top
9. Condenser duty, QC = (R –hD)D or

 QC 
hD    H1
 D  Q = (85x10 3
-0)41.2 = 3 460 800 kJ/h
R   C
H1  h D
10. Reboiler duty, QR = (hW-S)W
QR = (hW-S)W = (5 x 103 –[-64x103])58.8 = 4 057 200 kJ.h
129
Locating  S
Draw a straight line from  R through F to intersect the
vertical line at xW
130
Example 11.6-2
∆R
W
F
D
-64 x103kJ/kmol
∆S
131
Stepping off trays for the rectifying section
From V1 vertically to 45o

line, horizontally across to
equilibrium line and
vertically back to saturated
liquid line, to give L1.
Connect L1 to V1 using a tie

line. From L1 to R
intersecting the saturated ∆R
vapor line to give
V2.Repeat until a tie line V7 V6 V5 V V V V
4 3 2 1
crosses over the line ∆RF∆S. W L7 L6 L5 L4 L3 L2 L1

F
D
∆S
132
Stepping off trays for the stripping section
Draw a line from ∆S through
L7 up to the saturated vapor
line to give V8.
From V8 vertically to 45o

line, horizontally to
equilibrium line and
vertically back to saturated
liquid line to give L8.
∆R
Connect L8 and V8 using a
V12 V11 V10 V9 V8 V7 V6 V5 V V V V
tie line. 4 3 2 1
WL12 L11 L10 L9 L8 L7 L6 L5 L4 L3 L2 L1

Repeat until a tie line F
D
touches W or exceed W.
∆S
No. of theoretical stages =
no. of tie lines = 11.9 stages
133
MINIMUM REFLUX RATIO,
Rmin
Rmin occur when the line

∆RF∆S coincides with the
tie line that passes
through F
Get a tie line that passes
through F and extend that
line to intersect the
vertical line xD to get ∆Rmin
∆Rmin

 QC  W
 hD    H1 F
 D min Δ H
Rmin 

 Rmin 1 D
H1  h D Hh 1 D
134
MINIMUM STAGES, Nmin
Nmin is obtained when

the operating lines are
vertical since R and S
are at infinity.
Nmin = 5.9 stages
W
F
D
135
PARTIAL yD
CONDENSER
Distillate product, VD – vapor

with the composition yD
Condensed liquid/reflux, L0,

which is in equilibrium with y
have the composition xo D
x0
Partial condenser = 1 stage ∆R
V6 V5 V4 V V V V
3 2 1 D
W L6 L5 L4 L3 L2 L1 L0
F
∆S
136
PARTIALLY
VAPOURISED FEED, zF
F with the composition zF lies

on the tie line LF (composition
= xF) and VF (composition =
yF)
By trial-and-error, locate the

point F so as to satisfy the
inverse lever rule: zF
VF FL F
 F
VF VF
LF FVF W
LF LF F
137
7. Multicomponent Distillation
 Introduction
 Equilibrium data
 Boiling point, dew point and flash distillation
 Key components
 Total reflux
 Minimum reflux ratio
 Operating reflux ratio
 Short cut method for number of stages
138
7.1 Introduction
139
7.1 Introduction
F  D W (1)
Fx F  Dx D  Wx w (2)
Where
F is the entering feed (mol/h)
D is the distillate (mol/h)
W is the bottoms (mol/h)
140
7.1 Introduction
Material balance over dashed-line section: Vn 1  Ln  D (3)
A balance on component A: Vn 1 yn 1  Ln xn  DxD (4)
141
7.1 Introduction
Solving for yn+1, the enriching-section operating line is
Ln Dx
yn 1  xn  D (5)
Vn 1 Vn 1
Since Vn 1  Ln  D, Ln / Vn 1  R /( R  1)and equation becomes
R x
y n 1  xn  D (6)
R 1 R 1
where R  Ln / D = reflux ratio = constant.

The eqn. (1) is a straight line on a plot of vapor composition versus liquid
composition.
142
7.1 Introduction
The slope is Ln / Vn 1 or R /( R  1) . It intersects the y=x line (45º diagonal

line) at x  x D . The intercept of the operating line at x = 0 is y  xD /( R  1) .
The theoretical stages are determined by starting at xD and stepping off the first
plate to x1. Then y2 is the composition of the vapor passing the liquid x1.
In a similar manner, the other theoretical trays are stepped off down the tower in
the enriching section to the feed tray.
143
7.1 Introduction
Equation for
stripping section
Material balance over dashed-line section: Vm 1  Lm  W (7)
A component A balance: Vm 1 ym 1  Lm xm  Wxw (8)
144
7.1 Introduction
Solving for ym+1, the stripping-section operating line is
Lm Wx
ym 1  xm  W (9)
Vm1 Vm 1
Again, since equimolal flow is assumed, Lm  LN = constant and

Vm 1  VN
= constant,
L  Veqn. (2) is a straight line when plotted as y versus x,
m m 1
with a slope of . yIt 
intersects
Wx / Vthe y = x line at x = xw.
W m 1
The intercept at x = 0 is .
145
7.1 Introduction
146
8.2 Equilibrium data
For multicomponent systems which can be consideredideal, Raoult's Law
can be used to determine the composition of the vapor in equilibrium with
the liquid.
p A  PA x A , pB  PB xB , pC  PC xC , pD  PD xD
p A PA PB PC PC
yA   xA , yB  xB , yC  xC , yC  xC
P P P P P
In hydrocarbon systems, bacause of the nonidealities,

y A  K A xA , y B  K B xB , yC  K C xC , y D  K D xD
PB = Vapor pressure of pure B PA = Vapor pressure of pure A

pB = Partial pressure of B p A = Partial pressure of A
147
148
Relative volatility,  i
Ki K K K K
i  ,  A  A ,  B  B ,  C  C  1,  D  D
KC KC KC KC KC
The values of K i will be stronger function of temperature than the values of  i
149
7.3 Boiling point, dew point and flash distillation
(a) Boiling point (Bubble point calculation)
For a mixture of A, B, C and D with C as the base component,

 yi   K i xi  K C   i xi  1.0
The calculation is trial and error as follows :

First, a temperature is assumed and the values of  i are calculated from values of
K i at this temperature
The value of is calculated from K C  1.0/   i xi
The temperature corresponding to the calculated value of K C  1.0/   i xi
The temperature corresponding to the calculated value of K C is compared with
the assumed temperature
If the values differ, the calculated temperature is used for second trial
150
7.3 Boiling point, dew point and flash
distillation
After the final temperature is known, the vapor composition is calculated from
 i xi
yi 
( i xi )
(b) Dew point (dew point

calculation)
For dew point calculation, which is also trial and error,
 y   1   yi 
 xi   i        1.0
 Ki   KC   i 
The value of K C is calculated from K C   y /  i 
After the final temperature is known, the liquid composition is calculated from
y / i
xi 
 y /  i 
151
Example 11.7-1 Boiling Point of a Multicomponent Liquid
A liquid feed to a distillation tower at 405.3 kPa abs is fed to a

distillation tower. The composition in mol fraction is as follows:
n-butane (xA = 0.4), n-pentane (xB = 0.25), n-hexane (xC = 0.20),
n-heptane (xD = 0.15). Calculate the boiling point and the vapor
in equilibrium with the liquid.
152
distillation
• First, a temperature of 65 C is
o
•
assumed.
The K values are read from Fig.
11.7-2.
• Using component C as the base
component.
• The calculated value of Kc is 0.2745 corresponding to 69 oC.

•Using 69 oC for second trial, a temperature of 70 oC is
• Using 70 oobtained.
C for third trial, the calculation shown in the Table gives final calculated
value of 70 oC, which is bubble point.
 i xi
• The value of yi yi 
  i xi  153
calculated by
(c) Flash distillation
• Defining:
( 1  f)  L/F as the fraction of the feed
vaporized.
( 1  f)  L/F as fraction of the feed remaining
as liquid.
• Making the component I balances
f 1 x
yi  xi  iF
f f
where
yi  composition of component i in the vapor
154
distillation
(c) Flash distillation
• For
equilibrium
yi  K i xi  K C i xi where i  Ki / KC
f 1 x
yi  K C i xi  xi  iF
f f
• Solving for xi and summing for all components,
xiF
 xi    1.0
f  K C i  1
• This equation is solved by trial and error:
f fraction
 First assuming a temperature if the
vaporised has been set.
 When the  xi values add up to 1.0, the
proper temperature has been chosen.
 The composition of the vapor yi can be obtained
from
yi  K C i xi
155
Example
Example 10.5
The system acetone(1 )/acetonitrile(2)/nitromethane(3) at 80˚C and 110 kPa

has the overall composition, zi = 0.45, z2 = 0.35, z3 = 0.20.
Assuming that Raoult’s law is appropriate to this system, determine L, V,

{x1}, and {y1}. The vapor pressures of the pure species at 80˚C are:
P1sat = 195.75 P2sat = 97.84 P3sat= 50.32 kPa
Solution 10.5
First
Do a BURL P calculation with {zi} = {xi} to determine Pbubl . By Eq.
(10.2),
Pbubl = x1P1sat + x2 P2sat + x3 P3sat

= (0.45)(195.75) + (0.35)(97.84) + (0.20)(50.32) = 132.40
kPa
156
Example
Second
Do a DEW P calculation with {zi} = {yi} to find Pdew. By Eq. (10.3),
1
Pdew   101.52kPa
y1 y3
 y2 
P1sat P2sat P3sat
Since the given pressure lies between Pbubl and Pdew. the system is in
the two-phase region, and a flash calculation can be made.
By Eq. (10.11), Ki = Pisat / P: whence,
K1 = 1.7795 K2 = 0.8895 K3 = 0.4575
157
Example
Substitute known values into Eq. (10.17):
 0.451.7795   0.35 0.8895   0.20 0.4575 1

1  0.7795V 1  0.1105V 1  0.5425V
Solution for V by trial yields:
V = 0.7364 mol
Whence, L = 1 - V = 0.2636 mol
Equation (10.16) shows that each term on the left side of Eq. (A) is an
expression for v1. Evaluation of these terms gives:
y1 = 0.5087 y2 = 0.3389 y3 = 0.1524
158
Example
 Then by Eq. (10.10), x1 = y1 / K1 whence,
x1= 0.2859 x2 = 0.38 10 x3 = 0.3331
 Obviously, Σi yi = Σi xi = 1. The procedure of this example is valid

regardless of
the number of species present.
 Flash calculations can also be made for light hydrocarbons with the
data of Figs.
10.13 and 10.14.
 The procedure here is exactly as described in Ex. 10.5, where Raoult’s

law applied.
 With T and P specified, the K-values for light hydrocarbons as given by

Figs. 10.
13 and 10. 14 are known, and V. the only unknown in Eq. (10.17). is
found by
trial.
159
7.4 Key components in multicomponent distillation
 Light key (L)-The components separated which is more
volatile.
 Heavy key (H)
 Light Component -The component more volatile than light

key and will be
present in the bottoms in small amounts
 Heavy Component- The component less volatile than
heavy key and will be
present in distillate in small amounts
160
7.5 Total reflux for multicomponent distillation
Total reflux - Minimum number of theoretical stages/steps,

Nm
From Fenske equation 11.4-23
When applied to the heavy key H and the light key L,

log  x LD D / x HD D  x LW W / x HW W  
Nm 
log L ,av 
where
x LD  mole fraction of light key in distillate
x LW  mole fraction in bottoms
x HD  mole fraction of heavy key in distillate
x HW  mole fraction in bottoms
161
The average value of  L of the light key,

 L ,av   LD LW
where
 LD  at the top temperature (dew point)
 LW  at the bottom temperature
Distribution of other components
To determine the distribution of concentration of other component in

the distillate and the bottoms at total reflux,
xiD D x D
  i ,av  m HD
N
xiW W x HW W
162
Example 11.7-2 Calculation of Top and Bottoms Temperature and Total Reflux
The liquid feed of 100 mol/h at the boiling point given in Example 11.7-1 is fed to a
distillation tower at 405.3 kPa and is to be fractionated so that 90 % of the n-
pentane (B) is recovered in the distillate and 90 % of the n-hexane (C) in bottoms.
Calculate the following:
(a) Moles per hour and composition of distillate and bottoms.
(b) Top temperature (dew point) of distillate and boiling point of bottoms.
(c) Minimum stages for total reflux and distribution of other components
in the distillate and bottoms.
163
(a) Moles per hour and composition of distillate and bottom
Material balance are made for each component with n - pentane ( B) being the
light key ( L) and n - hexane (C ) as heavy key ( H )
Overall Balance :
F  D W
For component B, the light key,

x BF F  0.25(100)  25.0  y BD D  x BW W
Since 90% of C is in the bottoms and xCW W  0.90(20)  18.0, y CD D  2.0
For first tria l, assumed no component D in the distillate and no light A in the bottoms.
 mole A in distillate  y AD D  0.40(100)  40.0
 mole D in bottoms  x DW W  0.15(100)  15.0
164
• Moles composition of distillate and

bottoms.
165
7.5 Total reflux for multicomponent
distillation
(b) Top temperature (dew point) of distillate and boiling point of
bottoms.
For dew point of
distillate:
• A value of 67 oC will be estimated for
• first K
The trial.
values are read from Fig.
• 11.7-2.
The α is calculated.
• The following values are calculated:
• The calculated value Kc is 0.2627, which is very close to 67 oC.
• The final temperature is the dew point.

166
(b) Top temperature (dew point) of distillate and boiling point of
bottoms
For the bubble point of the
bottom:
• A temperature of 135 C is assumed for
o
the first trial.

• Calculate:
 i xi
 yi   K i xi  K C   i xi  1.0 and yi 
  i xi 
• A second trial using 132 oC gives the final temperature as

shown as below:
• The calculated value Kc is 1.144, which is close to the value at 167

132 oC.
(c) Minimum stages for total reflux and distribution of other
components
The proper  values of light key L (n - pentane),
 LD  2.50
 LW  2.04
 L ,av   LD LW  2.50(2.04)  2.258
log  0.349  64.5 / 0.031 64.5 0.507  35.5 / 0.070  35.5 

Nm 
log 2.258
 5.404 theoretical stages (4.404 theoretical trays)
For component A,
 A, av   AD AW  6.73  4.348  5.409
x AD D x D
  A, av  m HD   5.409
N 5.404 0.031(64.5)
 1017
x AW W x HW W 0.507(35.5)
168
(c) Minimum stages for total reflux and distribution of other
components
Overall balance on A,
x AF  40.0  x AD D  x AW W
x AD D  1017 x AW
Solving, x AW W  0.039
x AD D  39.961
For the distribution of component D,

 D,av  0.385  0.530  0.452
xDD D x D 5.404 0.031(64.5)

  D ,av  m HD   0.452
N
 0.001521
x DW W xHW W 0.507(35.5)
xDF F  15.0  xDD D  xDW W
Solving, xDD D  0.023

xDW W  14.977
169
• The revised distillate and bottom compositions

are as follows:
• Hence, the moles of D in the distillate are quite small, as are

the moles of A in the bottom.
170
• Using distillate compositions, recalculate the dew point assuming
67 oC gives a calculated value of Kc = 0.2637.
• This is very close to that of 0.2627 obtained when trace

amount od D in the distillate was assumed as zero.
• Thus, the dew point =

67 oC.
• Repeating the bubble point calculation for the bottom assuming
132 oC, a calculated value of Kc = 0.138, which is close to value of
132 oC.
• Thus, the bubble point = 132 oC.
171
7.6 Minimum reflux ratio
Shortcut method for minimum reflux ratio
Underwood' s Shortcut Method

x Assumptions:
1  q   i iF
i   Constant molar overflow
 i xiF  Constant relative
Rm  1  
i 
volatility
To solve for Rm
• The value θ of is first obtained by
trial and error.
• This value of θ lies between the
value of light key and the heavy key,
which is 1.0.
• Using this value of θ, the value of Rm is obtained
directly.
172
7.7 Number of stages
Shortcut method for number of stages at operating ratio
173
Shortcut method for number of stages at operating ratio.
Kirkbride
methods
To estimate the number of theoretical stages above and below the
feed which can be used to estimate the feed stage location
Ne  x  W  x LW 
2

log  0.206 log  HF    
Ns  x LF  D  x HD  
where
N e  number of theoretical stages above the feed plate
N s  number of theoretical below the feed plate
174
Example 11.7-3 Minimum Reflux Ratio and Number of Stages at Operating Reflux Ratio
Using the conditions and results given in Example 11.7-2, calculate the following.
(a) Minimum reflux ratio using the Underwood method
(b) Number of theoretical stages at an operating reflux ratio R of
1.5Rmin using the Erbar-Maddox correlation
(c) Location of feed tray using the method of Lirkbride.
Example 11.7-2 Calculation of Top and Bottoms Temperature and Total Reflux
The liquid feed of 100 mol/h at the boiling point given in Example 11.7-1 is fed to a distillation
tower at 405.3 kPa and is to be fractionated so that 90 % of the n-pentane (B) is recovered in the
distillate and 90 % of the n-hexane (C) in bottoms.
175
(a) Minimum reflux ratio using the Underwood
method
The temperature to use for determining the values of  i is average between
67  132
the top of 67 o C and the bottom of 132o C   99.5o C
2
The K i values obtained from Figure 11.7 - 2 and the  i values and distillate and
feed compositions are as follows :
176
With q  1.0 for feed at boiling point,
 i xiF
1 q  
i 
5.20(0.40) 2.30(0.25) 1.00(0.20) 0.467(0.15)
11  0    
5.20   2.30   1.00   0.467  
This is trial & error, so a value of   1.210 will be used got first trial ( must between 2.30 and 1.00)
This and other trials are shown below :
The final value of   1.2096 is obtained

Solvinf for Rm ,
 i xiF 5.20(0.6197 ) 2.30(0.3489) 1.00(0.031) 0.467(0.0004)
Rm  1      
 i   5.20  1.2096 2.30  1.2096 1.00  1.2096 0.467  1.2096
 Rm  0.395
177
(b) Number of theoretical stages at an operating reflux ratio R
of
R1.5R
 1.5Rmin using the Erbar-Maddox correlation
min  1.5(0.395)  0.593
R 0.593
  0.3723
R  1 0.593  1
Rmin 0.395
  0.2832
Rmin  1 0.395  1
From Fig. 11.7-3
N m / N  0.49
 N m / N  5.40 / N  0.49
Solving, N = 11.0 theoretical stages in

the tower.
178
(c) Location of feed tray using the method of Lirkbride
For the location of feed tray,

N  x  W  xLW 
2

log e  0.206 log  HF    
Ns  xLF  D  xHD  
Ne  0.20  35.516  0.0704  2 

log  0.206 log     
Ns  0.25  64.484  0.0310  
Ne
 1.184
Ns
Ne  Ns  N
1.184 N s  N s  11
N s  5.0
N e  6.0
 The feed tray is 6.0 trays from the top
179
7.8 Distribution of the components and plate-to-plate
calculation
The liquid in the reboiler is assumed to have the
composition of the bottom product and the vapor
leaving the reboiler is in equilibrium with it.
1. Calculate the vapor composition yw given the

liquid composition in the reboiler xw.
The temperature in the reboiler must be found
by trial. Assume 115 oC
Component xw Pwo (mm xwPwo yw= xwPwo /∑ xwPwo x1
Hg)
B 0.005 2040 10 0.0134 0.0119
T 0.744 861 641 0.8592 0.8388
X 0.521 380 95 0.1273 0.1497
1.000 746 0.9999 1.0004
Clearly the assumed temperature (115 oC ) was low

since the total pressure is only 746 mmHg. Repeat
at higher temperature.
180
calculation
2. Calculate x1 from yw . These are passing streams
and are related by the mass balance requirements
represented by operating line equations.
For stripping section:
ym = (L’/V’) x(m+1) – (W/V’) xw
For benzene: ymB = 1.221 x(m+1)B – 0.0011

For toluene: ymT = 1.221 x(m+1)T – 0.165
For xylene : ymX = 1.221 x(m+1)X – 0.0555
Example:
For benzene: ywB = 1.221 x1B – 0.0011

181
and x1B = (0.0134+0.0011)/1.221 =
calculation
At the ninth plate the following result was

obtained. The temperature = 95 oC
Component X8 Po (mm Hg) X8P Y8= x8P /∑ x8P X9

B 0.521 1186 618 0.745 0.611
T 0.420 476 200 0.241 0.33
X 0.059 199 12 0.014 0.057
1.000 830 1.000 1.0004
AND SO
ON!
182
7.9 Feed plate location
 xL  x  x 
    L    L 
 xH  f 1  xH  feed  xH  f
Where:
 xL 
  = Ratio light to heavy key on plate
 xH  f 1 above feed
 xL 
  = Ratio light to heavy key on feed
 xH  feed
plate
 xL 
  = Ratio light to heavy key in feed
 xH  f
 xL 
 
 xL 
 
Calculated using the same set of
and the operating line equations
 xH  f 1  xH  f 183
Summary – Course Outcomes
(CO)
6 - 11 Vapour-Liquid It is expected that students will be
Separation Processes able to:
Equilibrium relationship Describe batch distillation and
Simple distillation continuous fractional distillation
methods Design simple batch distillation
Binary fractional Design plate distillation column
distillation using using McCabe-Thiele
McCabe-Thiele method Design multi-component column
Multi-component using Fenske-Underwood-Gilliland
distillation correlation
.
184
Summary – Assignment 3
Thanks
185

Distillation

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Distillation

Hanapi Bin Mat, Ph.D

• Involved producing a vapour from a

PA = Vapor pressure of pure A

Calculate the vapor and liquid composition in equilibrium at 95 oC for

At 95 o C from Table 11.1 - 1 for Benzene,

Vapor-liquid equilibrium for A-B mixture e.g. benzene(A)-toluene (B)

 Heat a mixture of benzene-toluene at xA1 = 0.318 (boil at 98oC), first

 Non-ideal systems which will present more difficult separation

 An azeotrope is a liquid mixture which when vaporized, produces the same

xA = mole fraction of A in the liquid which is in equilibrium with y A phase

PA vapour pressure of pure A

At 85o C, for a system following Raoult's Law,

Constant molal overflow: V1 = V 2

Total material balance: L0 + V2 = L1 + V1

Unknown : x1 & y1 – solve simultaneously (graphically) between equilibrium line

=110 kmol xA1

110(0.3) + 100(0.4) = 110xA1 + 100yA1

lets xA1 = 0.3, yA1 = 0.4

1. Production of vapor by boiling the liquid mixture to be separated in a

2. Returning of a portion of the condensate to the still. The vapors

• Single stage binary distillation

• Vapor & liquid then separated

Unknown : x & y – solve simultaneously (graphically) between equilibrium line

L1 = Original moles charge L1 x dx

A mixture of 100 mol contaning 50 mol % n-pentane and 50 mol % n-heptane is

ln 100  x0.5 ydx

L1x1 = L2x2 + (L1-L2)yav

Note that by steam distillation, as long as water is present,

Then the vapor composition is

Temperature PA(water) PB(ethylaniline)

353.8 80.6 48.5 1.33

353.8 80.6 48.5 1.33 49.83

The boiling temperature = 99.15ºC since total pressure in this temperature

Multicomponents Multicomponent distillation

Rectification (fractionation) or stage distillation with reflux is

A total material balance: Vn 1  Ln 1  Vn  Ln

1. Feed enters the column somewhere in

2. Feed is liquid, it flows down to a sieve

3. Vapor enters the tray and bubbles

4. The vapor and liquid leaving the tray

5. The vapor continues up to the next tray

6. The concentration of the more volatile

7. The final vapor product coming

8. The remaining liquid from the

9. The liquid leaving the bottom tray

10. The vapor from the reboiler is sent

• Graphical method for determining the number of theoretical stages, N

A mathematical – graphical method for determining the number of theoretical trays

A balance on component A: Vn 1 yn 1  Ln xn  DxD (4)

Since Vn 1  Ln  D, Ln / Vn 1  R /( R  1)and equation becomes

where R  Ln / D = reflux ratio = constant.

Material balance over dashed-line section: Vm 1  Lm  W (7)

A component A balance: Vm 1 ym 1  Lm xm  Wxw (8)

Again, since equimolal flow is assumed, Lm  LN = constant and

The enriching and striping operating-line

Where the y and x values are the point of

Cold-liquid feed Superheated vapor

subcooled superheated partially vaporized

Total Reflux Ratio

One limiting values of reflux ratio is that of total reflux or R = ∞. Since R

Minimum number of trays can be obtained by returning all the overhead

• operating lines coincide with 45o line