Ahmed Mohamed Shafik Ali Attia professionalche@gmail.

com

Process & Operations Overview

On

Distillation Tower Design Considerations

By
Ahmed Mohamed Shafik Ali Attia
[email protected]
https://www.linkedin.com/in/ahmed-shafik-06612a20/
Ahmed Mohamed Shafik Ali Attia [email protected]

This document was developed as an intention to give an overview

on the design considerations of Distillation column.

It should enable design engineers to spotlight on the major criteria

to be considered, however, inevitably, thorough analysis and design
efforts to be imbedded to generate a properly design distillation
column.

I hereby would like to express my gratitude and thankfulness to the

great merciful Allah for granting me all the gifts, rewards and
abilities to produce such document and be able to share knowledge
with others.

I hope that this document can provide any support or help and in
case of any limitations or mistakes then all are mine and in case of a
wellbeing document and healthy information then it’s from the
great merciful Allah.

Ahmed Mohamed Shafik Ali Attia

Ahmed Mohamed Shafik Ali Attia [email protected]

Table of Content

 Introduction

 Specification

 Column Pressure

 VLE & Enthalpy

 Reflux and No. Of Stages Determination

 No. of theoretical stages Determination

 Tray Efficiency

 Tower Diameter Estimation

 Tray Type Selection & Design

 Feed location Determination

 Column Control Consideration

 Distillation Column in Fouling Services

 Useful References
Ahmed Mohamed Shafik Ali Attia [email protected]

Introduction
A distillation column is a series of equilibrium flashes with two feeds and two product streams
 Exiting liquid is at bubble point
 Exiting vapor is at dew point
Compositions obey the equation yi = Ki*xi

A subcooled liquid (“A”) is heated, its concentration remains constant until it reaches the bubble-point, when it
starts to boil (“B”).
The vapor evolved during the boiling has the equilibrium composition given by “C”.
This is approximately 50% richer in component A than the original liquid.
This difference between liquid and vapor compositions is the basis for distillation operations
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This technical guideline is mainly intended to use of process engineers involved in designing the
distillation column, therefore, this document will cover the design consideration of distillation column,
which includes:
 Distillation Design Procedure.
 Operating Pressure.
 Reflux ratio and Number of stages.
 Determination of Number of theoretical stages.
 TYPICAL DESIGN VALUES
 Feed location.

Specify Separation:

A material balance around the column is the first step in fractionation calculations.
In order to perform this balance, assumption of the product stream compositions must be made.

There are three ways to specifying desired product from the fractionators:
 A percentage recovery of a component in the overhead or bottom stream.
 A composition of one component in either product.
 A specific physical property, such as vapor pressure, for either product.
 In a multicomponent mixture, there are typically two components, which are as follows:
o Light Key (LK) Component: Defined as lightest component in the bottom product in a
significant amount.
o Heavy Key (HK) Component: Defined as heaviest component in the overhead
product in a significant amount.
Note: Normally, these two components are adjacent to each other in the volatility
list.
 For hand calculations, it is normally assumed for material balance purpose that all
components lighter than the light key are produced overhead and all components heavier
than the heavy product are produced with the bottom product
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Set Column Pressure:

Before any design calculations can be made on a fractionation problem, a tower operating pressure
must be determined.
Some considerations, as pressure increases, relative volatility mostly decreases, making separation more
difficult, the minimum number of stages increases, required exchanger sizes may decrease and eventually the
column may get mechanically more costly.

GPSA Engineering Data Book, Chapter 19

One of the primary considerations for operating pressure is cooling medium available for reflux
condenser.
The cooling media typically used are:
 Air: The least expensive cooling method. Design limits the process to an 11°C approach to
the ambient summer temperature.
 Cooling Water: The satisfactory temperature approach is 5 to 10°C.
 Mechanical Refrigeration: For process temperature below 35°C. This is the most expensive
cooling method from both a capital and operating cost (CAPEX / OPEX).
Example: If cooling water supply is at 32°C and return temperature of 40°C using above
guideline the condensing temperature is 45°C. For total condenser with a distillate
composition of C1, C2, C3 as 5/5/90%, the vapor pressure of the distillate @ 45°C is 23.3
kg/cm2a. Set the pressure of the reflux drum equal to or slightly above the vapor pressure
of the distillate at 45°C.
Generally, it is desirable to operate at as low a pressure as possible to maximize the relative
volatility between the key components of the separation.
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For a quick estimate of a gas oil/resid operation a pressure of 50 mm Hg at the overhead

line and a flash zone temp of 370°C may be used. However, if reducing the pressure
requires a change to a more expensive cooling method, this is the usually not a desirable
choice.
Whereas, in case of lighter hydrocarbon separation, say C2 from C3, use of a suitable
refrigerant is required when the distillate liquid temperature is lower than the cooling water
temperature. Designing such a column at the higher pressure will make:
 The refrigerant system smaller, but
 Reboiler duty and the column diameter will be larger.

In deciding the operating pressure of a column, a number of factors have to be considered in relation
to the total system.
A summary is provided below to indicate the advantages and disadvantages of operating a column at
higher pressure.
Advantages
 It increases the boiling points of the distillate and enables a cheaper cooling medium to be
used. If the cooling medium remains unchanged, it reduces the condenser area
requirements.
 It reduces energy costs in vacuum operation.
 It increases vapor density and vapor handling capacity. Leads to smaller column diameter
for pressure upto 3.5 to 10.5 Kg/cm2.
 It increases boiling points of liquids in the column for distillation of liquefied gases and
allows the use of cheaper construction materials.
 It reduces the size of pipes and valves for the vapor line.
 Below 1 atm, reduces air leakage into the system.

Disadvantages
 It decreases relative volatility and makes separation more difficult. It will therefore increase
reflux and stage requirements, and requires higher reboiler and condenser duties.
 It increases bottom product temperature and increases the risk of chemical degradation,
polymerization and fouling.
 Above 7 kg/cm2g, column shell thickness will probably increase, whereas below 7 kg/cm2g,
the effect is not as significant.
 Increases reboiler temperature, needs a more expensive heating medium or increase in
reboiler area requirement.
 It increases hazard potential if process materials are inflammable or toxic.
For mature technologies the operating pressures of the column have been standardized
except for some variation due to site condition, reference can be taken from similar
plant/equipment.
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CHOOSE VLE AND ENTHALPY DATA

 Choose correct VLE and enthalpy data ranges for property calculations.
 Choose correct methods for calculating properties.
 Inappropriate methods, models or data ranges can lead to poor results.
 Close boiling systems are especially finicky to converge.

Determine minimum reflux and minimum number of stage

Relation between Reflux Ratio and Number of stages:

The design of a fractionation column is a capital cost versus energy cost trade-off problem.
The primary parameters are the number of stages and the reflux ratio.
For most calculation, reflux ratio is defined as the ratio of the molar rate of reflux liquid divided by the
molar rate of net overhead product, R = L / D.
The desired separation can be achieved between the limits of minimum reflux and minimum stages.
The relationship between reflux ratio and number of stages for a given separation is shown below.
At minimum reflux an infinite number of stages are required while at total reflux a minimum number
of stages are required
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Determination of Minimum Number of Stages

Fenske’s equation can be used to calculate the minimum number of stages

If volatility varies widely, the approach of Winn is suggested, in which a modified volatility is used
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Determination of Minimum Reflux Ratio

The Underwood method can be used for calculating minimum reflux ratio.
The Underwood method assumes:
 Constant molar overflow, and
 Constant relative volatility at the average column temperature.

Once s is determined, the minimum reflux ratio is

Where,
Lo = Liquid Reflux Rate, kgmole/hr.
D = Distillate Product Rate, kgmole/hr
T = Correlating Parameter
a = Relative Volatility
i = any component
X = Liquid Rate, kgmole/h
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Set reflux ratio and calculate number of theoretical stages

It is customary to always add a certain safety margin above the minimum reflux level to avoid potential
errors from VLE estimation or from misdistribution at the desired reflux ratio.

The rule of thumb for R/Rmin which is regarded satisfactory as a general guideline is listed below

There are several considerations in deciding the reflux ratio; the following comments indicate the
effect of a change in the reflux ratio in relation to the number of stages.
 The higher the reflux rate, the higher the cost of condensing and reboiling. These make up
the bulk of the column operating costs.
 As reflux ratio increases, the number of stages decreases, but column diameter increases.
 Close to minimum reflux rate, small increases in reflux ratio will reduce the number of
stages considerably and therefore column height, but produce only a small increase in
column diameter.
 Further increases in reflux will have a smaller effect in the height reduction but greater
increase in column diameter.
The closest possible approach of design to minimum reflux requires accurate methods such
as vigorous stage wise calculations, developed by multiple cases on computers.

Determination of Number of theoretical stages:

The number of theoretical stages required for a given separation at a reflux ratio between minimum
and total reflux can be determined from Erbar and Maddox Correlation.
This correlation relates the ratio of minimum stages to theoretical stages to the minimum reflux ratio
and the operating reflux ratio as shown below:
We have calculated
 Minimum Reflux Ratio = Rm = (Lo/V) m
 Minimum number of stages = Sm
 R = (Lo/V) = Reflux Ratio.
 Knowing Sm/S from the graph below we can calculate S = Number of stage
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Adjust actual reflux for feed vaporization if necessary

The Erbar and Maddox correlation is based on bubble point feed.
For a feed stream between the bubble point and dew point the following relationship adjusts the vapor
rate from the top tray for non-bubble point feed.

V = Vapor rate, kg mol/hr

D = Overhead product rate, kg mol/hr
F = Feed rate, kg mol/hr
HVF = Vaporized feed stream enthalpy, Kcal/Kg mol
HBP = Bubble point feed stream enthalpy, Kcal/Kg mol
QC = Condenser duty Kcal/hr
LO = Liquid condensed in a partial condenser, Kg mol/h
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SELECT A TRAY EFFICIENCY

 Overall = # theoretical trays / # actual trays
 Point = (yout – yin) / (yeq – yin)
 Murphree = point efficiency, but over entire tray

GPSA Engineering Data Book, 12th ed, pg. 19-15

CALCULATE TOWER DIAMETER

Estimate tower diameter using rules of thumb

 “Heat Factor” of Q/d^2 = 350,000, duty in BTU/hr and diameter in feet
 “General Factor” of (R+F)/d^2 = 250, flows in BPD and diameter in feet

Refine diameter estimate with software tools such as KGTower and SULCOL.
Ahmed Mohamed Shafik Ali Attia [email protected]

DETERMINE TRAY TYPE

One of the most prominent hardwares used for mass transfer is tray.
Tray columns are widely used in various types of mass transfer operations.
All the simulation results, which predict a certain number of theoretical stages, can be converted to actual trays
depending upon tray efficiency for a particular service.

In any conventional tray vapour rises through the liquid pool on the tray deck and then disengages from the
liquid in the space above the deck. Liquid enters the tray from a downcomer above and leaves via a downcomer
below.
Conventional Tray has three functional zones:
1. Active area for mixing vapour and liquid: This is the zone where mass transfer occurs.
2. Vapour space above the active area: This is the zone in which liquid is separated from vapour.
3. Downcomer between trays. This zone has two functions, first moving liquid from one contacting tray
to another and second disengaging vapour from liquid.
Each of these zones takes up vertical and horizontal space in the tower.

Comparison between Common Conventional Trays

Factors Sieve Tray Valve Tray Bubble-Cap Tray Dual-Flow Tray
1 Capacity High High Moderately High Very High
2 Efficiency High High Moderately High Least
3 Turndown ~50% ~25-30% 10% Least
4 Entrainment Moderate Moderate High Low to moderate
5 Pressure Drop Moderate Moderate High Low to Moderate
6 Cost Low ~1.2 times sieve trays ~ 2-3 times of sieve trays Least
7 Maintenance Low Low to Moderate Relatively High Low
8 Fouling Tendency Low Low to Moderate High: Tends to collect Solids Extremely Low
9 Effects of Corrosion Low Low to Moderate High Very Low
Some information
10 Design information Well Known Proprietary, but readily available Well Known Available.Instability can occur in
large dia. (>8 feet)
Often used
Extremely low Liquid flow & Where Capacity revamps, Highly fouling and
11 MainApplication when turndown Where high turndown is required
leakage must be minimized corrosive services
is not critical
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DETERMINE TRAY SPACING

Use the table below as a guide for initial estimates.

Use KGTower or SULCOL software to rate a given internals type and tray spacing.

DETERMINE # OF TRAY PASSES

Use the table below as a guide for initial estimates.

Use KGTower and SULCOL to rate a given number of tray passes.

TYPICAL DESIGN VALUES

 Jet and downcomer flood < 85%.
 Downcomer backup of clear liquid < 40% of tray spacing plus weir height.
 Downcomer exit velocity < 1.5 ft/sec.
 Dry tray drop < 2” of liquid or < 15% of tray spacing.
 Total tray drop < 0.1 psi per tray.
 Weir load < 80 gpm/ft for one pass and < 120 gpm/ft for two or more passes.
 Head loss under downcomer of 0.06” to 1.0”.
 Weir height of 2” to 3”.
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Determination of feed location

Once a base case tower has been simulated, optimization studies on trays vs. reflux, feed tray location,
etc. can be carried out. One criterion often used for optimum location of the feed tray is to try and
match the feed composition as closely as possible to a corresponding tray composition.
The approximate feed location can be determined by the ratio of the total number of theoretical
stages above and below the feed plate from following equations:
 Fenske’s Equation
 Kirkbridge’s Equation
 Akashahetal’s Correction

 Fenske’s Equation
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DISTILLATION COLUMN CONTROL

1. REFLUX RATIO
The reflux to a structure top is used to management the top heat range thereby manages the
cleanliness of the expense item.
The quantity of reflux compared to the item is known as the ‘Reflux Ratio’.
An example of this is as follows:
The expense fluid from a distillation column is separated into 4 m3 hourly reflux and 2 m3 hourly item.
Therefore:

In general, the higher the reflux amount, the less the number of containers needed for a given
separating.
The reflux amount is normally managed by a heat range operator in the fumes store which functions a
management device in the reflux push release. An increase in structure top heat range will cause the
device to start, improving the reflux amount, and vice versa.

2. TEMPERATURE GRADIENT
Temperature (and pressure) management of a distillation structure will regulate the cleanliness of the
items.
The management of top heat range is as mentioned above in ‘reflux’.
Control over the supply inlet heat range and that of the reboiler are also very essential.
Again, if supply and bottom temperature ranges are too great, too much hefty fumes will rise up the
structure and put side-stream items off-spec.
This condition, along with great reflux amount will again cause to surging and inadequate separating.
Opposite conditions can cause to fluid hunger across the containers and again, a very disappointed
process will outcome.
The cautious management of top heat range, supply and reboiler temperature ranges, together with
stress management, will provide the preferred heat range information across the structure.
Remember!!!! Changes in stress will impact the steaming points of the elements in the feedstock. The
fumes demands therefore, will also be affected and again, if the management factors are wrong, the
program will be ineffective.
Examples:
 High top heat range will outcome in hefty elements in the expense item.
 Low top heat range will outcome in a less hefty top item.
 High supply heat range will provide bulkier side-streams and vice-versa.
 High reboiler heat range will produce bulkier soles item and pass bulkier vapours up the
structure to impact the side-streams.
 Increased stress in the program will provide less hefty elements in the expense LIQUID item
and reduce its Initial Boiling Factor, whereas the FBP is managed by the structure top heat
range.
It can be seen that cautious, precise management of the factors is very essential to experience the
needed qc of the items.
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Also, with respect to the cleanliness of the side-streams, management of the burning towers’ vapor
supply is very essential.
A further point is, that high-water content in the raw supply will cause stress deluges as the water
vaporizes in the structure. The raw oil should be as water free as possible.

VACUUM DISTILLATION TOWER OVERHEADS SYSTEM

In the above plan, the outer lining place condenser is a ‘Total Condensing’ unit. This means that all
liquids that can be compacted are modified to fluid. Due to this, a machine is established in the
structure the stage of which relies on the degree of moisture build-up or condensation permitted to
take place. This is managed by the stage of distillate and how much of the condensing surface place is
protected. The fluid stage and therefore the quality of condensing surface place available will decide
the stage of machine (Absolute Pressure) of the program.
The PRC is therefore managing the available condensing place on the chilling pipes.
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Increasing overall stress (decreasing vacuum), will start the management device, the fluid stage in the
condenser will fall thus introducing more condensing place to the fumes. More fumes will reduce and
therefore the stress will fall returning again – and vice-versa.

A small quantity of non-condensable fumes will tend to develop up in the structure and the outer lining
place condenser which, if permitted to develop up, will gradually eliminate the machine.

The ejector is used to eliminate the non-condensable which are approved into the separator after
moving through the ejector condenser which condenses the ejector vapor – thus helping to maintain
the machine, while the uncondensed fumes are fed via a check-valve or management device to
environment or width program.

The barometric closure cycle maintains a head of fluid which will prevent the machine taking fumes
returning out of the separator.

Distillation Columns in Fouling Service

Designing distillation columns in fouling service requires first an understanding of the fouling
mechanism, the process in which the fouling occurs, and behavior of the process when the fouling is
present.
An understanding of these items needs to be developed in advance of designing mass transfer
equipment for fouling service.
The challenges of fouling columns can result in;
 Increase energy consumption due to heat transfer and efficiency issues.
 Reduced column capacity, which may lead to production loses.
 Increased down time for cleaning and disposing of fouling wastes.
 Potential need for the use of chemical additive.
 General Guidelines
Fouling service in a distillation column is a broad term that encompasses many fouling phenomena.
The fouling phenomena can be localized in either the vapor phase or liquid phase. It the fouling is
localized in the liquid phase an inhibitor can be utilized.

Fouling phenomena can include;

 Vaporization of volatile components
 Polymerization
 Condensation
 Sedimentation / Precipitation / Crystallization
 Foaming
 Chemical Reaction
 Corrosion
Complex fouling problems are a result of a combination of two or more of these phenomena occurring
at the same time, such as in an ethylene caustic tower. They are nearly always mutually reinforcing.
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Factors that assist fouling phenomena can include;

 Residence time
 Stagnate zones
 Sharp transitions
 Emulsion issues
Consideration must also include the fact that fouling gets worse over time. Fouling is not static.

Fouling Mechanisms
A- Vaporization of Volatile Component
In many applications fouling can result if the volatile components are allowed to vaporize.
This fouling is found in refinery vacuum and de-asphaltene oil towers and ethylene quench oil towers.
If the process is placed on recirculation without the addition of fresh feed with volatile material, the
column can foul as the volatile components are removed.
In one example an ethylene quench oil tower was placed on circulation and viscosity of the bottoms
product increased beyond its pour point. The unit was shut down and required several days of off-line
cleaning.
B- Polymerization
Polymerization is the linking of double bonds to form long chain molecules. Examples of polymerization
include, polyethylene, polypropylene, polystyrene, poly butadienes and polyMMA.
These products are undesirable in the monomer distillation column.
These products can lead to reduced capacity and unit outages.
C- Condensation
Condensation is a reaction where two or more small molecules combine to from large, stable structure
molecules. Extreme condensation is the formation of coke at high temperature and long residence
times. Coke forms when thermal cracking removes hydrogen and light material from the fluid. A layer
of coke is left behind. Thermal cracking can occur in both the gas phase and the liquid phase. However,
the most common situation is liquid-phase cracking when low liquid rates extend residence time in
high-temperature operations.
Examples of condensation can be found in ethylene furnace transfer lines to the quench oil tower and
in refinery vacuum towers
D- Sedimentation / Precipitation / Crystallization
Sedimentation is the accumulation of solids that are deposited in low velocity areas in process
equipment.
The equipment can include heat exchangers, tower distributors, distillation trays, random packing, and
structured packing.
If the trays are fouled below the feed point the cause might be sedimentation.
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Many processes contain suspended solids, which can settle out on the mass-transfer surface.
Products of sedimentation can include salts, metal oxides, catalyst fines, and coke fines.
Precipitation and crystallization of dissolved salts can occur when process conditions become super
saturated, especially at mass transfer surfaces.
Ammonia salt deposition resulting from both water vaporization and direct solid deposition from the
gas phase is a common refining problem.
Sometimes the deposits formed do not adhere strongly to the surface and are self-limiting, the thicker
a deposit becomes, the more likely is to be removed by the fluid flow and thus attain some asymptotic
average value over time.

Sedimentation fouling is strongly affected by velocity and low temperature, however a deposit can
bake on a surface and become very difficult to remove.
Precipitation and supersaturation are fouling issues. Certain salts such as calcium sulfate are less
soluble in warm water than cold. If such a stream encounters a wall at a temperature above that
corresponding to saturation for the dissolved salt, the salt will crystallize on the surface.
Crystallization will begin at especially active points (nucleation sites) such as scratches and pits, often
after a considerable induction period and then spread to cover the entire surface. The buildup will
continue as long as the surface in contact with the fluid has a temperature above saturation. The scale
is strong, adherent and can require vigorous mechanical or chemical treatment for cleaning.

The following processes may cause super saturation:

 Evaporation of solvent
 Cooling below the solubility limit for solution with normal solubility, solubility increases with
temperature.
 Heat above the solubility of solutions with inverse solubility such as; CaCO3, CaSO4,
Ca3(PO4)2, CaSiO3, Mg(OH)2, MgSiO3, Na2SO4, Li2S04 and Li2Co3 in water.
 Mixing of streams with different composition.
 Variation of pH, which affects the solubility of CO2 in water.
 Ammonia salt deposition in refining.
 Additionally, solidification fouling can occur due to cooling below the solidification
temperature of a dissolved component, such as solidification of wax from crude oil.
Knowing the properties of the fluid and suspended solid, flow conditions and mixing effects one can
develop guidelines to predict sedimentation of solids from liquids.

E- Foaming System
Some systems have a propensity for fouling in the form of foaming.
In many systems an operating froth can be observed on the liquid phase.
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In distillation systems, the decrease in surface tension as equilibrium temperature rises promotes
foaming. High gas velocities allow liquid to be entrained into the vapor phase.
In non-foaming systems liquid disengagement from the vapor stream is relatively easy.
Foaming makes liquid disengagement from vapor flow difficult.
When foaming becomes severe it can lead to a reduction in capacity and loss of efficiency. In order to
counter this effect distillation equipment that operate in foaming systems are run a lower vapor and
liquid rates to reduce the amount of froth generated.
Sometimes anti-foam additives are added to distillation columns to decrease the amount of foam
generated in the column. There are drawbacks to using anti-foam chemicals. Sometimes they may
contaminate the end product and produce product that is does not meet production specifications.
F- Chemical Reaction
In distillation desired or undesired chemical reactions can occur. In an ethylene caustic tower there are
competing chemical reactions. The caustic absorbs the CO2 (desired) by electrostatic interactions and
Van der Wall attraction.
The acetaldehydes can be polymerized by the caustic (undesired) to form first a yellow oil polymer,
and then a red oil polymer by aldol condensation reactions, which can then lead to emulsions.
G- Corrosion
When corrosion occurs the increase surface roughness may promote fouling from the other fouling
mechanisms.
Ahmed Mohamed Shafik Ali Attia [email protected]

USEFUL REFERENCES

 Kister, H.Z., Distillation Operation

 Kister, H.Z., Distillation Design
 GPSA Handbook, Chapter 19, “Fractionation”
 Branan, Carl, Rules of Thumb for Chemical Engineers, Chapter 3, 4th
ed., 2005, Gulf Publishing.
 Watkins, R.N., Petroleum Refinery Distillation
 Don’t Gamble with Physical Properties for Simulations, Eric Carlson,
Chemical Engineering Progress, October 1996, pp. 35-46.
 Seader, J. D., Ernest J. Henley, and D. Keith. Roper. Separation Process
Principles: Chemical and Biochemical Operations. 3rd ed. Hoboken, NJ:
Wiley, 2011. Print.
 "ENCYCLOPEDIA OF CHEMICAL ENGINEERING EQUIPMENT." Distillation
Columns. N.p., n.d. Web. 11 Feb. 2015.
 Biegler, L., Grossmann, I., Westerberg , A., 1997, Systematic Methods of
Chemical Process Design, Prentice Hall.
 Bravo, Jose L. and James K. Fair. "Distillation Columns." Chemical
Engineering Progress January 1990: 19-Willis, M. J., Selecting a
Distillation Column Control Strategy, Department of Chemical and
Process Engineering, University of Newcastle, 2000.