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DiStillation PDF
DiStillation PDF
DiStillation PDF
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SOURCES OF EQUILIBRIUM DATA
• Henry’s Law
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SOURCES OF EQUILIBRIUM DATA
• K-Value – vapor-liquid equilibrium ratio
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Sources of Equilibrium Data
• K-Value (DePriester Chart Fig. 13-9 ChE HB 8th
ed.)
SOURCES OF EQUILIBRIUM DATA
• Relative Volatility
Example
• What is the relative volatility of C6H6 / C7H8
system @
A) T1 = 102˚C
B) T2 = 106˚C
106
102
0.21 0.38
0.09
SIMPLE BATCH
(DIFFERENTIAL) DISTILLATION
SIMPLE BATCH
(DIFFERENTIAL) DISTILLATION
• Batch Distillation – is where the separation of
components of an initial volume of liquid mixture
(i.e., a batch charge) is carried out in a heated
vessel (pot). The vapors may pass through a
rectifying column on their way to condenser. The
condensed stream is collected and/or refluxed.
• In simplified form of batch distillation, no
rectification or reflux is provided, and the batch
material is boiled and condensed
SIMPLE BATCH
(DIFFERENTIAL) DISTILLATION
• The batch charge is constantly changing in
composition and volume. Therefore, batch
distillation is not a steady state process.
SIMPLE BATCH
(DIFFERENTIAL) DISTILLATION
• Initial Mixture,
A1 = FxF
F
B1 = F(1-xF)
• Final Mixture
A2 = WxW
W
B2 = W(1-xW)
EQUATIONS
• 1) Overall Material Balance
• 2) Component Balance
A1 = FxF A2 = WxW
B1 = F(1-xF) B2 = W(1-xW)
EQUILIBRIUM OR FLASH DISTILLATION
• Flash Distillation – consists of a vaporizing a
definite fraction of the liquid in such a way
that the evolved vapor is in equilibrium with
the residual liquid, separating the vapor from
the liquid, and condensing the vapor.
• In this process, the feed, F is continuously
heated where the potential vapor is allowed
to be in intimate contact with the liquid at a
certain temperature and pressure.
EQUILIBRIUM OR FLASH DISTILLATION
• This mixture is then allowed to pass through a
pressure reducing valve, a vapor-liquid
equilibrium results, and the two phases are
separated.
EQUILIBRIUM OR FLASH DISTILLATION
EQUILIBRIUM OR FLASH DISTILLATION
• Graphical Method
EQUILIBRIUM OR FLASH DISTILLATION
Sample Problem
• A liquid mixture containing 736 lbs toluene & 156
lbs benzene is distilled until the mixture attains a
Bpt of 106˚C.
A) Calculate the composition of the residue &
distillate
B) At what temperature does distillation begin?
C) Suppose the above mixture was subjected to
equilibrium distillation with same amounts of
products obtained in diff. distillation, find the
product & composition
D) Compare differential and flash distillation
Flash Calculation
• Objectives:
A) Calculate the composition of the liquid and
vapor streams
B) Determine the amount of the liquid and
vapor streams
Flash Calculation
• OMB:
Flash Calculation
• CMB: ith component
• Since
Flash Calculation
• Make sure that the feed will form 2 phases at
the given T & P
A) Determine PBUBBLE & PDEW
– If P > PBUBBLE then
If you are sure that the two phases will form, solve for
McCabe Thiele Method
Rectifying Section: L D
Equilibrium y x x
Operating line V V D
curve Slope=L/V=R/(R+1)<1
q-line
yN
q z F
y x
q 1 q 1
Stripping Section: L B
yB Operating line y x xB
V V
45° line Slope=L/V=(VB+1) /VB
xB x=zF xD
Overhead vapor Reflux drum
q=1 q>1 1 Distillate
Reflux
Rectifying section stages
L* 2
0<q<1 L
L+V x=y Feed
f Feed Stage
5. and 6. 7.
3. 4.
equilibrium equilibrium equilibrium
equilibrium
curve curve curve
curve
y y y y
Rmin/(Rmin+1) R/(R+1)
Feed Location for the McCabe-Thiele Method
Equilibrium Equilibrium
curve curve
1 1
y 2 y 2
3
yN 3 yN
4
4 5
yB yB
6
xB xD xB x=zF
x=zF xD
Feed stage located one tray too low. Feed stage located one tray too high.
Optimum Feed Location for McCabe-Thiele
Equilibrium
curve
y 2
yN
3
yB
xB xD
x=zF
4 Solution:
Step 1: From xD locate x1 and y1 drawing a horizontal line
to the equilibrium condition for stage 1.
yB Step 2: Find y2 drawing a vertical line to the rectifying OL
locate the mass balance condition between x1 and y2.
xB xD Step 3: From y2 draw a horizontal line to the equilibrium
x=zF condition for stage 2 to locate x2.
Step 4: Return to step 2 and cycle through steps 2 and 3 until
xi <zF. Draw subsequent vertical lines to the stripping section OL.
Step 5: End after predetermined number of stages, or when x i is
less than xB.
Minimum Number of Stages for McCabe-Thiele
Equilibrium
curve
y 2
yN
3
yB
xB x=zF xD
By returning all the exiting vapor as Although this is the minimum number
reflux and all the exiting liquid as boilup of stages, no product is produced (note
the operating lines have slope of one. the feed must then
go to zero).
Minimum Reflux for McCabe-Thiele
Equilibrium
curve
yN
yB
xB x=zF xD
yN
yB
xB x=zF xD
Construction:
Step 1: Plot equilibrium curve and 45 degree line.
1 The equilibrium curve is found using:
0.9 x
y
0.8 1 x 1
0.7 Step 2: Plot given compositions (F, B, and D)
Step 3: Draw q-line from LF and VF. Use
0.6
L L L LF L LF
y 0.5 q 0.7
F F F
0.4
to find q. Then plot the q-line using:
0.3
q z
0.2 y x F 2.333x 2
0.1
q 1 q 1
Construction:
Step 5: From Rmin=0.333 and R=3Rmin we have R=1
And the slope of rectifying section OL is 0.5
1
Step 6: Draw the line with slope 0.5 which is the rectifying
0.9 section OL.
Step 7. Draw the stripping section operating line from the
0.8
Bottoms composition to the intersection of the rectifying section
0.7 OL and the q-line.
0.6
Solution:
y 0.5 Step 1: From xD locate x1 and y1 drawing a horizontal line
to the equilibrium condition for stage 1.
0.4
Step 2: Find y2 drawing a vertical line to the rectifying OL
0.3 locate the mass balance condition between x1 and y2.
Step 3: From y2 draw a horizontal line to the equilibrium
0.2
condition for stage 2 to locate x2.
0.1 Step 4: Return to step 2 and cycle through steps 2 and 3 until
xi <zF.
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Results:
x Feed at stage between 2 and 3.
5 stages (minimum stages = 3.2)
65
xB=0.05% benzene
Example: Determination of N and xB for McCabe-Thiele
Given:
100 Kmol/hr of a feed of 60% benzene and 40% heptane is to be separated by distillation. The distillate is to be 90% benzene and
The bottoms 10% benzene. The feed enters the column as 30mol% vapor. Use R 3 times the minimum. Assume a constant relative
Volatility of of 4 and that the pressure is constant throughout the column at 1atm.
1
Minimum number of stages is determined by stepping off
0.9 between the equilibrium curve and the 45 degree line.The
0.8 result is 3.2 stages.
0.7
0.6
y 0.5
0.4
0.3
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
x
McCabe-Thiele Method: Subcooled Reflux
Distillation Column
Total condenser
(subcooled reflux)
Reflux Distillate
Feed
Boilup
Partial reboiler
Bottoms
H
P1
T V
P2
Pcr Bubble point line
HV
L V
L
T
Tm Tb X1(V) XD(L)
0
dH C PdT V1 T dP
XB 1
McCabe-Thiele Method: Partial Condenser
Distillation Column
(partial condenser)
Partial condenser
Vapor
Distillate
Overhead vapor
Reflux
Feed
Boilup
Partial reboiler
Bottoms
Vapor
yD Partial condenser
Distillate
Overhead vapor
Equilibrium
curve
q-line Reflux
yN
q z
y x F Feed
q 1 q 1
Boilup
yB Bottoms
xB x=zF
McCabe-Thiele Method: Multiple Feeds
Distillation Column Total condenser
(multiple feeds)
Reflux Distillate
Feed 1
Feed 2
Boilup
Partial reboiler
Bottoms
The McCabe-Thiele method for cascades can be applied to systems with more than
two sections. Here, we show a cascade with 2 feeds: A 3 section cascade.
Feed 2 Feed 2
Boilup Boilup
Bottoms Bottoms
McCabe-Thiele Method: Multiple
Total condenser
Feeds
The flow rates above Feed 1 are constant due to constant molar
overflow (CMO). The feed changes the slope depending on the
feed condition. Flow rates in the intermediate section are constant,
but change when Feed 2 is introduced. Overhead vapor Reflux drum
Reflux Distillate
Feed 1
Feed 2
Boilup
Partial reboiler
y
Rectifying Section: Bottoms
Operating Line
Equilibrium
Constant Slope (CMO)
curve
yN Feed 1 introduced
Intermediate section:
Operating Line
Constant Slope (CMO)
yB Feed 2 introduced
Stripping Section:
Operating Line
Constant Slope (CMO)
xB xD
McCabe-Thiele Method: Multiple Feeds
Example: Feed 1 a saturated vapor of composition zF1, q=1 q>1
and Feed 2 a saturated liquid of composition z F2
0<q<1 L L*
L+V x=y
V LL
q=0 q
F
q<0 V*
x=zF
y Saturated vapor
Rectifying Section:
Operating line
Equilibrium
Slope=L/V=R/(R+1)<1
curve
yN
Intermediate section:
Operating line
Slope=L’/V’
yB Saturated liquid
Stripping Section:
Operating line
Slope=L/V=(VB+1) /VB
xB x=zF2 x=zF1 xD
McCabe-Thiele Method: Side Stream
Occasionally a cascade is configured such that an
intermediate side stream of intermediate composition
is removed from the column.
Reflux Distillate
How do we analyze this configuration?
Ls
Use the multiple mass balance envelopes and
assume a constant molar overflow condition. Feed
Boilup
Vn1y n1 Ln x n Dx D
Ln D Ls
yn1 xn x
Vn1 Vn1 D
Feed
For L and V constant from
stage to stage, then: Boilup
L D
y x xD Operating line above side stream Bottoms
V V
McCabe-Thiele Method: Side Stream
If we perform a material balance in the light key
around the stages above the side stream
including the side stream and condenser:
Reflux Distillate
V y L x L x Dx
n 1 n 1 n n s s D
Ls
Which we can rearrange to find:
Feed
Ln L x Dx D Boilup
yn1 xn s s
Vn1 Vn1
Bottoms
For L and V constant from
stage to stage, then:
L' L x Dx
y x s Operating line below side stream
V V
xx
s
McCabe-Thiele Method: Side Stream
Side Stream:
y Liquid withdrawn
Rectifying Section:
Operating line
Equilibrium
Slope=L/V=R/(R+1)<1
curve
yN
Intermediate section:
Operating line
Saturated liquid feed Slope=L’/V
yB
Stripping Section:
Operating line
Slope=L/V=(VB+1) /VB
Total condenser
xB x=xs xD
Distillation
x=zF
Overhead vapor Reflux drum
Boilup
Stripping section stages N
Partial reboiler
Bottoms
McCabe-Thiele Method: Open Steam
Total condenser
Consider the cascade shown on the left:
Distillation
In this example, the reboiler is replaced by a Overhead vapor
source of hot steam or an inert gas. In this case,
the vapor entering the bottom stage of the column Rectifying section stages 1 Reflux Distillate
has no light key and so yB is zero, although xB is 2
non-zero.
Feed Feed Stage
Distillation
Overhead vapor Reflux drum
xB x=zF xD
Rectifying section stages 1 Reflux Distillate
2
xB xD
x=zF
x
Equilibrium y
curve
1 x 1
y
yN Rectifying Section: R 1
Operating line y x xD
R 1 R 1
Slope=L/V=R/(R+1)<1
yB Stripping Section: L B
Operating line y x xB
Slope=L/V=(VB+1) /VB
V V
45° line
q z
q-line y x F
xB x=zF q 1 q 1
xD
McCabe-Thiele: Minimum Reflux
To carry out the algebraic method we need to determine the slopes of the operating lines
algebraically. This can be done finding the intersections between the q-line and equilibrium
curve, and the q-line and the rectifying section operating line.
x
y
yD 1 x 1
q z
y x F
y q 1 q 1
yB
q z x
y x F
45° line q 1 q 1 1 x 1
xB x=zF xD
McCabe-Thiele: Rectifying Section
Operating Line
The slope of the operating line for the rectifying section with minimum reflux can be determined
from the rise over run. We can then also find the minimum reflux from this slope.
q z x
y x F
q 1 q 1 1 x 1
yD
y D yq Rmin
xD xq Rmin 1
y
q 45° line
From the minimum reflux, and R/Rmin we can
determine the reflux R.
R
slope
R 1
xB x x=zF xD
q
McCabe-Thiele: Rectifying Section
Operating Line
We can find the intersection of the operating line and the q-line to determine the stripping
section operating line:
q z R 1
y x F x xD
q 1 q 1 R 1 R 1
yD
R
slope
R 1
yQR
45° line
From the minimum reflux, and R/Rmin we can
determine the reflux R.
1 1. Alpha = 4, R=Rmin
2. Alpha=4 R=2Rmin
y 2 3. Alpha=4 R=4Rmin
4. Alpha=4 R=20Rmin
5. Alpha=1.1 R=3Rmin
yN
3
yB
xB xQR xD
x=zF
MULTISTAGE MULTICOMPONENT
DISTILLATION
Key and Nonkey Components
Key components are the two components in a
mixture that characterize the degree of
separation or that may provide the basis for a
separation to be achieved.
MULTISTAGE MULTICOMPONENT
DISTILLATION
Light Key : The more volatile of the two key
components. Present in both the distillate and
bottoms product, and recovered predominantly
in the distillate product.
1
MINIMUM NUMBER OF STAGES
• Relative Volatility
• Let i = LK and j = HK
MINIMUM NUMBER OF STAGES
MINIMUM NUMBER OF STAGES
• is obtained from one of the following
1)
2)
3)
4)
MINIMUM NUMBER OF STAGES
• is obtained from one of the following
5)
Steam (Inert) Distillation
• A component with a high boiling point can be
distilled at a lower overall temperature by
introducing steam into the still pot. However,
the steam must be immiscible with the
mixture being distilled. Assuming the heat of
vaporization comes from the steam, the total
pressure in the still pot is the sum of the vapor
pressure of the high boiler (A) and the steam.
Steam (Inert) Distillation
• The ratio of the moles of the component A to
the moles of steam is
Number 1
The difference between stage operation (A) and a
continuous phase contact operation (B) is that
A) (A) is co-current flow while (B) is counter-
current flow
B) (A) yields discrete concentration changes while
(B) yields infinitesimal concentration changes
C) (B) yields discrete concentration changes while
(A) yields infinitesimal concentration changes
D) An ideal (B) yields equilibrium concentration
while (A) does not
Number 2
One hundred moles per hour of solution
containing 80 moles of A, the rest B is subjected
to a simple continuous distillation. D moles of
distillate containing 72 moles A is obtained. If A
is five times more volatile than B, the
concentration of A in the distillate is
A) 0.85 C) 0.533
B) 0.80 D) none of these
Number 3
The temperature of the solution in Problem 2 as
distillation progresses at constant operating
pressure is
A) Increasing
B) Decreasing
C) Constant
Number 4
If the enthalpy of saturated vapor at 200 F
referred to 32˚F is 1300 Btu/lb while the
enthalpy of saturated liquid (Cp = 1) referred to
0˚F is 400 Btu/lb, then the latent heat of
vaporization of the component at 200˚F is
A) 900 Btu/lb C) 868 Btu/lb
B) 932 Btu/lb D) none of these
Number 5
Desorption is another term for
A) Dephlegmation
B) Stripping
C) Flash distillation
D) rectification
Number 6
In a simple batch distillation, the boiling point of
the distillate product compared to the residue is
A) The same
B) Lower
C) higher
Number 7
When the feed to the rectifying column is a
saturated liquid, the feed line is
A) Vertical
B) Horizontal
C) Inclined to the left
D) Inclined to the right
Number 8
The distillation process involves
A) momentum transfer
B) Mass transfer
C) Heat transfer
D) Heat and Mass transfer
Number 9
A liquid mist 45% benzene and 55% toluene by
weight is to be fed to a fractionating column at a
rate of 5000 kg/h. The feed rate in kg-moles/hr
is
A) 58.74
B) 58.80
C) 48.80
D) 28.846
Number 10
A binary solution, where A is a lower boiler,
exhibiting a maximum boiling point, is subjected
to flash distillation. If the feed has a
concentration in A less than the azeotropic
point, the concentration of the distillate will be
A) Higher in A
B) Higher in B
C) same
Number 11
The unit operation by which miscible liquids are
separated from one another through heat and
mass transfer is
A) Extraction
B) Sedimentation
C) Distillation
D) Filtration
Number 12
When the relative volatility of two miscible
components is close to 1.00, the components
can be separated by
A) Simple fractionation
B) Batch distillation
C) Extractive distillation
D) Low pressure distillation
Number 13
The degrees of freedom associated with a
ternary distillation process, according to the
Gibb’s phase rule, is
A) 2
B) 3
C) 4
D) 5
Number 14
Vacuum distillation is resorted to in order to
A) Reduce the number of trays in the column
B) Use thinner shell plates for the column
C) Avoid high feed and reboiler temperatures
D) Obtain more bottom products
Number 15
To improve the degree of separation of the more
volatile component from the less volatile
component through distillation, the chemical
engineer may, without changing the other
variables,
A) Increase the feed temperature
B) Reduce the column pressure
C) Increase the reboiler temperature
D) Increase the column pressure
Number 16
Increasing the operating pressure of a
distillation column
A) Does not make a difference in components
separation
B) Makes separation difficult
C) Sharpens separation
D) Requires less heat in the feed heater
Number 17
A reboiler provides heat to the
A) Top
B) The intermediate reflux
C) The feed
D) The bottom of a distillation column
Number 18
When the molal latent heat of vaporization of
the binary system is a very much dependent on
concentration, the most appropriate method to
use to determine the number of ideal stages is
A) Fenske-Underwood Method
B) McCabe-Thiele Method
C) Ponchon-Savarit Method
D) Lewis-Matheson Method
Number 19
Open steam binary rectification may be applied
with success if the less volatile component is
A) Water
B) Alcohol
C) Benzene
D) acetone
Number 20
At minimum reflux ration, the number of plates
is
A) Minimum
B) Infinite
C) Maximum
D) Between minimum and maximum
Number 21
In a vacuum distillation column the vacuum is
usually created by a
A) Steam ejector
B) Vacuum pump
C) Compressor
D) Centrifugal pump
Number 22
The relative volatility of the mixture at the
azeotropic point where the solution exhibits
minimum boiling point is
A) Less than 1
B) Equal to 1
C) Greater than 1
Number 23
The ease or difficulty of separating components
by distillation is determined by the
A) Relative volatility
B) Viscosity
C) Mole fraction
D) Weight fraction of the components
Number 24
A debutanizer is a
A) Heat transfer equipment
B) Mass transfer equipment
C) Fluid transfer equipment
D) Size reduction equipment
Number 25
In distillation, the cooled liquid stream returned
to the column to cool a plate or stage is called
A) Reboil
B) Reflux
C) Feed
D) bottoms
Number 26
A binary mixture of 2 moles benzene and 8
moles toluene will boil at
A) 110˚C
B) 110˚F
C) 105˚C
D) 102˚C
Number 27
McCabe-Thiele method to determine the
theoretical number of stages may be applied
with acceptable result if
A) The components have different boiling points
B) The system follow Trouton’s Rule
C) The components have high relative volatility
D) Heat losses and heat of solution are
negligible
Number 28
The distribution coefficient of n-hexane at 10
atm abs and 200˚C is
A) 2.6
B) 1.4
C) 0.9
D) None of these
Number 29
The theoretical minimum reflux ratio in a
distillation column is enough if the column has
A) 1 plate
B) 10 plates
C) 100 plates
D) An infinite number of plates
Number 30
The physical separation of components in a
miscible mixture by simultaneous evaporation
and condensation is
A) Absorption
B) Extraction
C) Drying
D) Distillation
Number 31
In batch open steam distillation, the solution to
be open steam distilled should be
A) Miscible in water
B) Completely immiscible in water
C) Slightly miscible in water
D) Containing large non-volatile impurities
Number 32
In a distilling column, the highest pressure will
be at
A) The top
B) The feed plate
C) The bottom
D) Between the feed plate and the top
Number 33
The unit operations by which the lighter
components in a multicomponent solution of
volatile liquids are separated from the heavier
components is called
A) Absorption
B) Drying
C) Distillation
Number 34
In distillation where there are two components
and both components are found in both phases,
only one variable such as liquid phase
concentration can be changed independently if
the pressure is fixed and the temperature and
vapor phase concentration will follow. This
statement is ______
A) True
B) False
Number 35
A heat transfer equipment to convert vapor to
liquid is an/a
A) Evaporator
B) Reboiler
C) Condenser
D) Still
Number 36
For a mass transfer to take place, there must be
A) concentration gradient
B) More than two components involved
C) Heat present
D) Enthalpy change
Number 37
A 50% by weight benzene-toluene mixture is fed
to a column at 180˚F and 1 atm. The condition
of this feed is
A) Saturated liquid
B) Saturated vapor
C) Sub cooled liquid
D) Mixture of liquid and vapor
Number 38
A distillation column with a partial condenser is
composed of 7 theoretical stage in the rectifying
section and 8 theoretical stages in stripping
section, If the overall plate efficiency is 60%,
then the actual feed plate is the
A) 11th
B) 13th
C) 12th
D) 8th from the top
Number 39
Using the Antoine’s Equation, the vapor
pressure of tetrahydrofuran at 80˚C is estimated
to be ______ torr.
A) 2000
B) 1518
C) 1173
D) 2562
Number 40
The total actual number of plates of the
distillation column of Problem 38 is
A) 13
B) 22
C) 26
D) 15
Number 41
Strictly speaking, the relative volatility of most
ideal binary solution is
A) Not affected by temperature
B) Greatly affected by temperature
C) Slightly affected by temperature
D) Greatly affected by pressure
Number 42
The temperature in a distilling column, from
bottom to top
A) Increases
B) Decreases
C) Maximum
D) Between minimum and maximum
Number 43
The primary reason why close steam is used in
an open batch distillation is to
A) Increase the number of degrees of freedom
B) Increase the operating temperature
C) Supply the heat needed by vaporizing liquid
D) Increase the operating pressure
Number 44
In a two-component flash distillation process,
when the operating pressure is specified, the
concentration of the distillate may be improved
in the more volatile component if
A) The operating temperature is decreased
B) The operating temperature is increased
C) The amount of distillate is increased
D) None of these
Number 45
If the HETP of the column of Problem 38 is 2 ft
then the height of the packed column is
A) 30 ft
B) 43 ft
C) 26 ft
D) None of these
Number 46
The percentage change in the boiling point of a
20-mole benzene-toluene solution when the
pressure is increased from 1 atm to 2 atm is
A) 10.5% increase
B) 25.5% increase
C) 25.5% decrease
D) None of these
Number 47
The recent availability of digital computers
resulted in the development of many analytical
expressions for the evaluation of K-values.
Which of the items below is a source of
analytical method of K-values?
A) NRTL
B) Wilson Equation
C) UNIQUAC
D) All of these
Number 48
The activity coefficient of a component in a non-
ideal liquid solution at low pressure is
approximated to be equal to
A) One
B) Vapor pressure multiplied by the
composition on the liquid phase in mole
fraction
C) Vapor pressure divided by the total pressure
D) None of these
Number 49
The approximate minimum number of stages for
a binary system wit relative volatility of 2.35,
fractionally distilled to yield compositions of
0.98 in the distillate and 0.045 in the bottoms is
A) 4.8
B) 7
C) 8.1
D) 12
Number 50
For nearly pure products in a stage operations,
the theoretical number of plate may be
estimated using the
A) Rayleigh equation
B) Fenske equation
C) Tiller-Tour equation
D) Murphree equation