DISTILLATION OF ETHANOL (DIST)

OBJECTIVES
Your company produces an aqueous solution of 20 mol% ethanol that requires further
purification before it can be sold on the market. The company plans to utilize an eight-stage
sieve-tray distillation column to further purify the ethanol. The company can sell the distillate if
its composition is more than 75 mol% ethanol and plans to reuse the bottoms stream if its
composition is less than 10 mol% ethanol. Before operating column, however, the company has
asked you characterize experimentally the column performance and utilize Aspen Plus
simulation software to assess the feasibility of the separation and to provide some
recommendations. Specifically, the company wants to investigate the effect of reflux ratio on
stream purity and ethanol recovery. For a fixed feed flow rate and reboiler duty, you are to
recommend an appropriate reflux ratio given the companys technical constraints and economic
considerations.
The company has requested you complete the following tasks:
i.
At total reflux, measure the overheads flow rate as a function of reboiler power and
determine the column flooding limit.
ii.
Measure tray, overheads, and reboiler compositions at total reflux and 75 % of flooding,
then utilize the McCabe-Thiele method to calculate the overall column efficiency and the
individual Murphree tray efficiencies.
iii.
Characterize experimentally the column performance at a feed rate F = 2 L/hr, reflux
ratio R = 5, and 75 % of flooding while feeding to the bottom of the column.
iv. Model the column performance with Aspen software at the conditions specified in (iii)
and discuss agreement between the experiment and model.
v. Utilize the Aspen model to recommend the appropriate R to obtain a distillate
composition xD 0.75 and a bottoms composition xB 0.10 at fixed F and Qreb.
BACKGROUND & THEORY
A significant amount of literature is dedicated to the theoretical treatment of heat and
mass transfer, thermodynamics, and hydraulics within distillation columns. These subjects are
covered at length in Chapter 21 of Unit Operations of Chemical Engineering by McCabe et al.
[1] and in Chapter 7 of Separation Process Principles by Seader et al.[2]. The following section
provides a brief overview of column flooding, the McCabe-Thiele graphical method, Murphree
tray efficiency, and vapor-liquid equilibrium (VLE) data for ethanol/water mixtures.
Column flooding
Figure 1 (from McCabe et al. p 704 [1]) is a schematic cutaway illustrating the normal
operation of a sieve plate. Liquid from the stage above flows through the downcomer onto the
DIST-1

stage below. As the liquid flows across the stage towards the overflow weir, it contacts the vapor
from the stage below rising through the holes in the sieve plate. The resulting frothy mixture

Figure 1: Cutaway depicting normal operation of a sieve tray. From McCabe et al. p 704 [1].

creates intimate contact between the liquid and vapor streams (and lots of area for mass transfer)
before the liquid flows over the weir and onto the next stage. In an ideal case, the liquid and
vapor phases are well mixed on a stage and no concentration gradients exist across the stage.
A pressure gradient between stage n+1 and stage n must exist to drive vapor flow through
the perforated tray and through the liquid. Similarly, the liquid flows through the downcomer and
across the tray due to a gradient in liquid head. Thus, the vapor velocity must exceed a minimum
velocity or else liquid will flow down through the holes and prevent vapor flow through them. In
this condition, called weeping, the vapor and liquid have limited contact and plate efficiency is
decreased. On the other hand, if the vapor velocity is too high, then liquid is entrained in the
vapor and transported to the stage above. Additionally, the pressure drop across a stage can be so
great that it drives liquid up the downcomer and onto the stage above. In this conditions,
generally called flooding, the plate efficiency drops and the pressure drop becomes very large.
Correlations to predict the flooding limit of sieve-tray columns can be found in McCabe et al. p
705 [1]. Normal operation falls between weeping and flooding where the vapor velocity is
high enough to create a frothy mixture but not high enough to cause entrainment.
In principle, measurement of column efficiencies and pressure drops can identify the
flooding limit. Because the column is glass, you can observe the physical behavior on the trays
and confirm flooding visually.
McCabe-Thiele method
Binary-component distillation can be analyzed using the McCabe-Thiele method to
predict theoretical column behavior. In this graphical method, equations of the operation lines in
the rectifying section (portion of the column above the feed) and stripping section (portion of the
column below the feed) are obtained by performing material balances over a control volume
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encompassing the relevant column section. Stages are numbered from top to bottom, with n and
m denoting the tray number in the rectifying and stripping sections, respectively.
Assuming constant molal overflow throughout the column, a material balance on the
more volatile component (ethanol) in the rectifying section relates the vapor concentration
entering stage n from stage n+1, yn+1, to the liquid concentration leaving stage n, xn:
x
R
y n1
xn D
R 1
R 1
(1)
where xD is the mole fraction of ethanol in the distillate, R=L/D is the reflux ratio, L is the
molar flow rate of liquid in the rectifying section, and D is the molar flow rate of distillate.
Similarly, a material balance on ethanol in the stripping section relates the vapor
concentration entering stage m, ym+1, to the liquid concentration leaving stage m, xm:
V 1
x
ym1 B
xm B
VB
VB
(2)
where xD is the mole fraction of ethanol in distillate, VB = V /B is the boil-up ratio, V is the
molar flow rate of vapor in the stripping section, and B is the molar flow rate of the bottoms
product.
The equation of the feed line is obtained by performing a material balance on the feed
plate:
q
1
y
x
xF
1 q
1 q
(3)
where y is the vapor ethanol mole fraction, x is the liquid ethanol mole fraction, xF is the
mole fraction of ethanol in the feed, and q is moles of liquid flow in the stripping section that
result from the introduction of each mole of feed. The value of q depends on the phase and
temperature of the feed.
Starting from the condenser (or from reboiler), one can step stages graphically and
calculate the composition of vapor and liquid on each plate using Eqs. (1)-(3) and equilibrium
data. The calculations progress until the concentration of the liquid matches with that of the
bottom product. This way one can calculate the number of equilibrium stages needed
theoretically (Nth). Comparison of Nth with the actual number of column stages, Nact, needed to
effect the same separation defines the overall column efficiency:
N th
ov
N actual
(3)
The overall column efficiency, therefore, compares the actual column performance to that of a
column where the liquid and vapor leaving each stage are at equilibrium. In practice, this rarely
happens, necessitating the use of Murphree tray efficiencies outlined below.
Murphree tray efficiency
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The Murphree tray efficiency, M, is defined by

y yn1
M n
y n yn1
where yn is the composition of vapor leaving stage n, yn+1

(4)
is the composition of vapor entering

yn
stage n, and
is the composition of vapor in equilibrium with the liquid leaving stage n. The
Murphree tray efficiency is, therefore, the change in vapor composition on stage n relative to the
change that would occur if the liquid and vapor leaving stage n were in equilibrium. This
provides a useful measure of how much mass transfer occurs on a stage.
The Murphree tray efficiencies can be used to characterize actual column behavior. In the
McCabe-Thiele graphical method, stage stepping can be performed without reaching the
equilibrium line. Instead, each step from the operating line only partially approaches the
equilibrium line, as described in McCabe et al. p 715. As a result, effecting a particular
separation necessitates more stages than if it the column were 100 % efficient.
Although Seader et al. outline some empirical and semi-theoretical models for predicting
tray efficiency (ref. [2] pp 297-82), analysis of liquid or vapor samples from each tray during
column operation enables direct calculation of tray efficiency according to Eq. (4). In practice,
liquid samples are easier to collect and analyze. Calculation of M for each stage from Eq. (4)
requires a relationship between the vapor compositions, y, and the liquid compositions, x, on
each stage. The operating line provides this relationship. Note that the calculation is significantly
simpler when the column operates at total reflux.
VLE data
McCabe-Thiele analysis and Murphree tray efficiencies both require VLE data describing
the distribution of ethanol and water between the liquid and vapor phases at various mixture
compositions. Reliable values of y and x for constructing an equilibrium curve are located in
Table VI of Cornell et al.[3]. The Aspen software also contains a built-in module for calculating
binary VLE data for non-ideal mixtures utilizing various property methods such as UNIQUAC
or NRTL [4]. You should know that both of these property methods were developed by Prof.
Prausnitz here at U.C. Berkeley in the Chemical Engineering department.
EXPERIMENTAL APPARATUS
The experimental apparatus for the distillation experiment consists of the distillation
column with its associated tanks, computer, and control console as well as the gaschromatography (GC) setup for measuring the composition of ethanol/water samples.
Distillation column and apparatus
Figure 2 shows a schematic of the distillation-column apparatus in S1 Gilman. The
equipment comprises a 50-mm diameter sieve-plate column made up of two glass sections and
each containing four sieve plates. The column sections are separated by a central feed section
DIST-4

and are arranged vertically for counter-current vapor-liquid flow. Also installed within the
framework are a reboiler, two 5-liter feed tanks, a peristaltic feed pump, a condenser, bottom and
top product receivers, a decanter, and a reflux valve.
The reboiler, situated at the base of the column, contains a flameproof immersion-heating
element. The column and the reboiler are insulated to minimize heat losses. In continuous

Figure 2: Schematic diagram of distillation apparatus. Solid lines correspond to flow

DIST-5

and dashed lines correspond to vacuum. Note that the vacuum lines are not connected in
S1 Gilman.

operation, the valve (V1) from the reboiler is open and bottom product flows from the reboiler
through the bottom product cooler to the bottom product receiver. It is possible to preheat the
feed by directing the feed through a heat exchanger where heat is transferred from product
leaving the reboiler at the boiling point. A level sensor inside the reboiler protects the heating
element from overheating due to low operating level and a sight glass allows the level in the
reboiler to be observed.
Vapor from the top of the column passes to a water-cooled coil-in-shell condenser. The
condenser incorporates a pressure relief valve to protect the system in the event of a blocked vent
and/or cooling-water failure. Cooling water enters the condenser at a regulated rate through a
variable area flowmeter (FI1) and the flowrate is controlled by diaphragm valve V5.
Condensate is collected in a glass decanter (phase separator). With valve V10 open,
condensate from the condenser passes directly through the decanter to the inlet of the reflux-ratio
control valve, which is 3-way solenoid actuated. Depending on the setting of the reflux timers,
condensate is directed by the reflux valve either back to the top of the column or to the top
product receiver (see reflux ratio control on page 11). When directed to the column, the reflux
passes through a U-seal where a valve (V3) can be used for measuring boil-up rate or for
draining the U-seal. The contents of the top product tank can be drained into the reboiler for reuse via valve V12.
Temperatures within the system are monitored by fourteen thermocouples located at
various positions. Thermocouples T1 to T8 are located in the column and measure the
temperatureoftheliquidoneachsieveplate.
The total pressure drop across the column is indicated on a U-tube manometer via taps in
the column fitted with isolating valves V6 and V7.
Liquid compositions are obtained by using a gas chromatograph (see pages 14-16).
Samples of feed, bottoms, and distillate can be withdrawn from the feed tank, valve V2, and
valve V3, respectively. There are 10-mL vials available on the counter north of DIST1 for storing
the liquid samples.
The glass column incorporates a total of eight sieve plates in two sections each containing
four plates as shown in Figure 3. Each plate contains a central support rod (E) and incorporates a
weir (F) and a downcomer (G) to create a liquid seal between successive stages. The U-tube (H)
achieves the liquid seal on the final plate in each section.
A pair of spouts is incorporated in the glass-column wall at each sieve plate (see Figure
3). One spout incorporates a temperature sensor to measure the liquid temperature. The second
spout incorporates a septum seal that allows a sample of liquid or vapor to be drawn by inserting
a hypodermic syringe through the seal. The septum heals when the syringe is withdrawn
preventing leakage. If the septum leaks, please notify the GSI immediately.
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Feed mixture from either of the feed tanks is pumped by the feed pump to the base,
center, or top of the distillation column. Feed-stage selection is achieved by adjusting valves VA,
VB, or VC. Note that the bottom feed point directs the feed mixture directly to the reboiler.

Figure 3: Schematic diagrams of the sieve plates in the column. The leftmost diagram
shows an entire section consisting of four plates, the middle diagram depicts liquid and
vapor movement through three plates, and the rightmost diagram shows a cutaway of a
single stage including the sample ports and thermocouple sensors.

DIST-7

Gas Chromatography Column

Ethanol/water liquid-mixture compositions are determined by using a gas
chromatograph (GC). Gaschromatography,illustratedinFigure4,involves asamplebeing
vaporizedandinjectedontotheheadofthechromatographiccolumn.Thesampleistransported
throughthecolumnbytheflowofaninert,gaseousmobilephase.Thecolumnitselfcontainsa
liquidstationaryphase,whichisadsorbedontothesurfaceofaninertsolid.TherearetwoGC
unitsinS1GilmantobeusedwhilerunningtheDIST1andDIST2experiments.

Figure 4: Schematic diagram of a gas chromatograph.

The carrier gas within the GC must be chemically inert. Commonly used gases include
nitrogen, helium, argon, and carbon dioxide. The choice of carrier gas is often dependent upon
the type of detector, which is used. In this case, the carrier gas is helium. The carrier-gas system
also contains a molecular sieve to remove water and other impurities.
For optimum column efficiency, the sample should not be too large, and should be
introduced onto the column as a "plug" of vapor; slow injection of large samples causes band
broadening and loss of resolution. The most common injection method is where a micro-syringe
is used to inject sample through a rubber septum into a flash vaporizer port at the head of the
column. The vaporized sample enters the column oven at a temperature of about 141C. For
these columns, you need only to inject 1-L samples. Too large of a sample will overload the
detector and lead to poor results.
As shown schematically in Figure 4, the raw result from the GC is simply two peaks that
correspond to ethanol and water. The PEAK software provided on the computers calculates the
area under each peak. Through a calibration, the relative peak areas are converted into mole
fractions to obtain composition measurements. Figure H-1 in Appendix H shows a calibration
relating mole fraction ethanol to peak-area fraction of ethanol for the GC units in S1 Gilman and
a sample size of 1 L. This calibration is good for ethanol mole fractions between 0.10 and
0.90. You are to use this calibration to convert your raw area fractions into compositions. This
calibration should be confirmed by running at least one known ethanol/water sample (i.e., 25 or
50 mol% ethanol). Detailed operating procedures for the GC column are listed in Appendix H.

DIST-8

SIMULATION
As part of your objectives you are asked to simulate the distillation column with
AspenOne V8.6 (Aspen) process-simulation software. Aspen is capable of solving the
necessary coupled mass and energy balances to predict the operation of numerous chemicalengineering unit operations such as flash drums, heat exchangers, reactors, pumps, columns, etc.
To simulate distillation of the ethanol/water mixture, Aspen must also make VLE calculations
utilizing appropriate property methods to calculate the requisite activities and fugacities in the
liquid and vapor phases.
In this particular case, simulation of the column with the Radfrac module is sufficient to
complete the objectives requested by the company. Note that you do not need to add in extra
units for the condenser, reboiler, or feed pump. For step-by-step instructions on constructing an
Aspen simulation of the column, see the Aspen tutorial uploaded to the bCourses website. The
simulation requires a number of inputs that are either directly measured in the experiment or can
be estimated from the experiment. The goal of the simulation is to predict the column outputs
(distillate and bottoms flow rate and purity) given the controllable inputs (feed flow rate and
conditions, number of stages, reboiler duty, reflux ratio). The only inputs in the Aspen simulation
not directly controllable are the Murphree tray efficiencies. However, you estimate these based
on column measurements at total reflux.
AspenOne V8.6 software is available on the computers in the Chevron Computing
Facility in Tan Hall. Additionally, discs are available for installation on your personal computer.
The discs must remain in lab at all times; ask your GSI for a copy to borrow during lab.
Installation instructions are located on the course website.
SAFETY
Review the Material Safety Data Sheets (MSDS) for ethanol and water. Although these
chemicals are common, it is NOT advisable to breathe or drink any quantity of the ethanol-water
mixture. It is also NOT advisable for the skin to be in contact with the mixture. In the event of a
spill or leak, DO NOT attempt to block or collect the holt liquid or vapor. Turn off the power to
the heater and immediately notify the GSI.
Although the column is designed to operate at one atmosphere, the student must always
be aware of the column pressure. Elevated pressure is an indication of high condenser
temperature and is accompanied by substantial venting of ethanol.
There are two primary safety issues while taking liquid samples. The liquid in the column
especially in the reboiler is HOT. At close to 90 C, there is a risk of scalding. Students
should wear proper PPE (gloves, goggles, long pants, closed-toed shoes) at all times. When
taking samples from each stage, the syringe plunger takes some strength to pull back. However,
pulling back too hard can result in the plunger coming out of the syringe and scalding liquid
spraying out. Additionally, take care not to pierce yourself with the sharp syringe.
PRE-LAB EXERCISES
DIST-9

1. Review the safety information described above. Go online and try to find some resources
about typical scalding times for various temperatures. Can the reboiler liquid scald you?
2. Construct an equilibrium y-x curve for ethanol/water mixture using either Aspen software
and an appropriate property method or the data given in ref. [3]. How do the various
methods compare?
3. Identify the azeotrope in your y-x diagram. What is the maximum composition of ethanol
theoretically obtainable in the distillate stream?
4. Why must the standardized samples of ethanol/water mixtures located with the GC units
not be opened for long periods of time?
5. Identify which valves need to be open/closed to operate at (i) total reflux and (ii)
continuous operation with feed to the bottom position.
6. Assume that the distillation column is initially operating at steady state. If you increase
the feed flow rate and all other valve settings remain the same, what will happen to the
temperature and composition of the bottoms? What change(s) must be made to return to
the original bottoms composition and steady-state operation at this higher feed flow rate?
The candidates for change include power to the heater and the flow rates of bottoms,
distillate, or reflux.
7. Assume that the distillation column is initially operating at steady state. If you then
increase the power to the heater and all other valve settings remain the same, what
happens to the distillate composition? Are there other important changes to the operating
condition? What change(s) must be made to return to the original distillate composition
and a steady-state operation at this higher power? The candidates for change include flow
rates of the bottoms, distillate, reflux, and the feed.
8. Assume that the distillation column is initially operating at steady state. If you decrease
the reflux flow rate and increase the distillate flow rate by the same amount, so that the
accumulator level remains constant, and all other valves settings remain the same, what
happens to the distillate composition? What change(s) must be made to return to the
original distillate composition and a steady-state operation at these new flow rates? The
candidates for change include power to the heater and the flow rates of bottoms or feed.
PROCEDURE
A. Column startup
During startup, your goal is to begin column operation at total reflux in a safe, controlled
manner. Before beginning this step, be sure that you are familiar with the valve locations and
overall column setup.

DIST-10

1. Make sure you have at least one full feed tank with sufficient ethanol/water mixture. The
feed-mixture composition should be 20 mol% ethanol. Verify the composition using gas
chromatography.
2. Check that all the proper valves are open/closed to operate at total reflux. The feed valves
VA-C should be closed, the bottoms valve V1 should be closed, etc.
3. Turn on the computer software and power up the control console and establish
communication between the two. The passwords for the computers are listed in Appendix
F.
4. Ensure the reflux-ratio controller is set to total reflux (i.e., power is off).
5. Open valve V5 to set the flow rate of cooling water to the condenser to about 3 L/min.
Important: Periodically check the rotameter to confirm the flow rate has not dropped
significantly
6. Turn on the reboiler power to 1.2 kW (dial reading ~6.0). Once froth and bubbling are
visible on trays, turn down the reboiler power to 0.75 kW (dial reading ~3.3).
7. Track the process temperatures during startup to determine when the column has reached
thermal steady state. This typically takes at least 30 min. When you are confident of
steady operation, move on to the determination of the column flooding limit.
8. At the end of startup each lab period, draw liquid samples from the reboiler and measure
its composition with the GC to ensure composition is as expected.
B. Determination of column flooding limit
The objective of this portion is to determine the flooding limit of the column at total

Q R

reflux by varying reboiler power

and, therefore, boilup rate
pressure drop P, overheads flow rate L, and tray hydraulics.

, and measuring column

1. With column operating at steady state and total reflux (likely from Part A), record the
reboiler power and begin performing measurements outlined below.
2. Note the hydraulic behavior (degree of foaming) on the stages with following descriptors:
none, gentle localized, violent localized, foaming gently over whole tray, foaming
violently over whole tray, or liquid flooding in column. Note it is possible that not all
trays will exhibit the same behavior.
3. Measure the column pressure drop with the manometer. If the tray observations indicate
liquid flooding, do NOT open the manometer. Zero manometer before each reading. To
take reading, open V6 then V7. To isolate manometer, close V7 then V6.
4. Measure overheads flow rate L by a timed-volume collection with a 100-mL graduated
cylinder. Open diversion valve V3 and close the green valve to the column to begin flow
to the graduated cylinder. Collect enough volume to ensure accurate volume
DIST-11

measurement, but do not divert the overheads for too long because it disturbs column
operation. Typically 1-2 min is sufficient.
5. By observing the tray temperatures, allow the column to return to thermal steady state
before repeating Steps 2-5 again to obtain duplicate measurements at each reboiler power.
6. Repeat Steps 2-6 for varying reboiler powers between ~0.4-1.0 kW. Allow adequate time
for the column to reach each new steady state (usually >15 min). Once flooding is
observed, only take one measurement and return the reboiler power to 0.75 kW or
whichever power you had planned next. If the column operates at flooding conditions for
too long, it will take a long time to recover for the next steady state.
C. Measurement of efficiencies at 75% flooding
To calculate the overall column efficiency, ov, and individual-tray Murphree vapor
efficiencies, M, at 75% of flooding, you must measure the composition of liquid samples from
each tray, the overheads, and bottoms during total-reflux operation. Tray temperatures should
also be recorded.
1. Begin (or continue) column operation at total reflux with the reboiler duty determined in
Part B to be 75% of the flooding limit (likely near 0.75 kW). In either case, wait the
appropriate amount of time for the column to reach thermal steady state, as indicated by
the tray temperatures.
2. Utilize the data-acquisition software in Table mode to record all thermocouple
temperatures. This enables you to later collect a temperature profile in the column.
3. Dispense and collect a liquid sample from the bottom of the reboiler using valve V2.
Careful the liquid is HOT! Samples should be collected into the small glass vials
provided on the counter to the north of DIST1. Save and label the sample for GC
analysis.
4. Beginning at Tray 8 and sequentially ascending the column, collect a liquid sample from
each trays sample port (see Fig. 3) utilizing the long-needled syringe provided near the
vials. DO NOT use the microliter syringes located at the GC units. When possible, guide
the syringe tip to the liquid by looking through the glass wall to locate where the tip is on
the tray. Save and label each sample for GC analysis.
5. Divert the overheads product to collection vial using valve V3 and the green valve as in
Step 4 of Part B. You need only collect enough for a sample; you do not need to perform
a flow-rate measurement.
6. After column returns to thermal steady state, repeat Steps 2-5 to obtain duplicate
measurements.
D. Steady-state column operation

DIST-12

The objective is to operate the column in continuous mode producing distillate and
bottoms products at a fixed reboiler power (likely 0.75 kW) and a feed rate of 2 L/hr. You
measure experimentally xD, xB, and L; D and B are calculated from these results.
1. Begin (or continue) column operation at total reflux with the reboiler duty determined in
Part B to be 75% of the flooding limit (probably 0.75 kW). In either case, wait the
appropriate amount of time for the column to reach thermal steady state, as indicated by
the tray temperatures.
2. Open the top of the peristaltic pump, place the plastic tubing inside it, and close it. Ask
you GSI if you have questions. Next, open the bottoms feed valve, VC, and turn the feed
pump on at 2 L/hr, commencing feed to the column. Utilize the calibration curve in
Figure G-1 to choose the appropriate dial reading for the feed pump. Inspect the feed line
to confirm that liquid is indeed flowing to the column. Quickly go to Step 3.
3. On the control console, change the reflux ratio to 5:1, initiating flow of distillate into the
top-product receiver. See Figure A-2 and Appendix B for instructions on setting the reflux
timer on the console.
4. Note the height of liquid in the level indicator on the front of the reboiler. Open gradually
the needle valve V1 at the reboiler exit and attempt to use V1 to attain a steady liquid
level in the reboiler. Frequent level checking and valve fine tuning are necessary during
the entire operation. Ideally, one teammate would serve as a dedicated reboiler-level
controller.
5. Observe the tray temperatures and reboiler liquid level to judge when the column has
reached steady state.
6. At steady state, dispense and collect a liquid sample from the bottom of the reboiler for
GC analysis.
7. Utilize either the data-acquisition software or pen and paper to record all tray
temperatures. This will be useful in analyzing and checking your data.
8. Measure the overheads flow rate L by a timed-volume collection. Open diversion valve
V3 and close the green valve to the column. Transfer a small amount of sampled liquid to
a vial for GC analysis of the distillate composition. Again, do not collect overheads for
longer than 1-2 min to avoid significant disruption to the steady state.
ANALYSIS & DESIGN
The following calculations and exercises form an outline of the analysis to be completed
on the experimental and simulation results. You can and should go beyond these calculations to
answer other questions relevant to the objectives. Keep in mind you may not be able to include
all of these results in the oral report. Select those results that you feel are most important to tell
the story.
DIST-13

1.

Plot the measured overheads flow rate, L, as a function of reboiler power. Does the trend
follow your expectations qualitatively and quantitatively? What are some possible
reasons for disagreement?

2.

Construct a McCabe-Thiele diagram for your column operation at total reflux and step off
stages between the measured bottoms and distillate compositions assuming 100 %
efficiency. Given the actual stages in the column, what is your columns overall
efficiency?

3.

Next, utilize the tray samples collected in Part C to construct a McCabe-Thiele diagram
describing the actual column performance. What are the Murphree tray efficiencies for
each of your trays? How do these tray efficiencies compare to the overall column
efficiency?

4.

Perform a mass balance around the distillation column with the data from Part D. Be sure
to take into account the error in each measurement. You have enough data for
redundancy. That is, you have measured more flow rates and compositions than
necessary. It is possible that both the component and overall balances agree, but it is
unlikely. Why not? Which measurements have the most uncertainty?

5.

Simulate in Aspen the column behavior under continuous operation at the conditions
listed in the procedure. Follow the instructions in the Aspen tutorial to initialize and run a
simulation. The goal here is to compare the Aspen-predicted column flow rates,
compositions, temperatures, etc. to those measured in the experiment. Which values agree
best? Which agree the worst? Does changing any inputs to the Aspen simulation result in
better agreement between experiment and simulation?

6.

Next, utilize the sensitivity analysis function in the Aspen simulation to predict the
behavior of the column at varying reflux ratio with all else held constant. From the
simulation data, identify the effect of reflux ratio on the column performance,
specifically, stream compositions and the ethanol recovery. Reason physically why the
trends look the way they do.

7.

Consider how you would have completed the same analyses from Questions 5 and 6
using the McCabe-Thiele graphical method. What steps would you have to take? Would
multiple iterations be necessary?

8.

Based on the trends elucidated in Question 6, recommend an ideal reflux ratio for column
operation that enables the company to meet their target composition specifications while
maximizing the ethanol recovery. Identify tradeoffs associated with changing reflux ratio.

REFERENCES
DIST-14

1. McCabe W.L, Smith J.C., Harriott P. Unit Operations of Chemical Engineering, 7th ed.;
McGraw-Hill: New York, 2005.
2. Seader J.D., Henley E.J., Roper D.K. Separation Process Principles, 3rd ed.; Wiley: New
York, 2011.
3. Cornell L.W., Montonna R.E. Ind. Eng. Chem. 1933, 25, 1331.
4. Smith J.M., Van Ness H.C., Abbott M.M. Introduction to Chemical Engineering
Thermodynamics, 7th ed.; McGraw-Hill: New York, 2005; pp 447-9

APPENDICES
Appendix A: Control Consoles
A control console is attached to the process unit by an umbilical cable. The individual
sections of the console with descriptions are shown in Figures A-1, A-2, A-3, and A-4.

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Figure A-1: Distillation-column main console. The various control panels within the
main console control the reflux timer (Fig. A-2), the reboiler heater (Fig. A-3), the feed
pump (Fig. A-3), and column/process temperature readings (Fig. A-4).

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Figure A-2: Power and reflux-ratio control panels.

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Figure A-3: Reboiler-heater and feed-pump control consoles.

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Figure A-4: Process and column temperature control consoles.

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Appendix B: Reflux-Ratio Control

The bottom of Figure A-2 shows the reflux-ratio timer on the control console. This sets
the amount and frequency of condensate flow returning to the distillation column. With the timer
switched off, all condensate is directed to the column (total reflux).
For example, if the reflux-ratio required is 2:1 and the total cycle time required is 21
seconds (arbitrary choice), then the reflux-ratio valve to the column directs condensate to the
column for 14 s then to the top-product receiver for 7 s. This cycle is repeated continuously until
different values are inserted to the controller or until the reflux control is switched off.
The time range and mode of the reflux-ratio timer can only be set when the electrical
supply to the timer is switched off. Switch off the reflux-control switch on the control console
(LED not illuminated). This switches off the power supply to the reflux-ratio timer. The refluxratio timer is now not controlling reflux flow (flow is continuous to the top of the column).
Because the controller has an internal battery, the display is still illuminated, and the controller
settings may be adjusted.
1.
Press the SET button on the reflux-ratio timer. The timer should be set to Cycle mode
(CY). If CY is not already set, use the button to cycle through the modes until CY is
displayed. (Not ICY).
2.
Press the SET key again.
3.
Select the time range required for CY+ (time to the receiver vessel: distillate).
4.
Press the SET key again.
5.
Repeat the time range setting for CY- (time to the column: reflux).
6.
Press SET to end time adjustment. To begin controller operation, switch on power to the
reflux-ratio timer using the reflux-control on/off switch.
Appendix C: Measuring Column Pressure Drop
The overall pressure drop over the column can be measured using the manometer. Before
taking a measurement, make sure to zero the manometer by relieving any pressure with the
pipette bulbs. Open V6 and V7 sequentially and take the pressure reading. When the reading is
complete, close both valves (first V7 then V6). This procedure reduces the risk of contamination
of the manometer water by ethanol. Also to prevent contamination, never open valves V7or V6
when flooding is occurring on the sieve plates (boil-up rate too high).

Appendix D: Collecting Liquid Samples

Samples for analysis can be taken from pertinent points in the system as follows:
Feed liquid from feed tank
Liquid in reboiler V2 (WARNING! Liquid at boiling point!)
Condensate, reflux or top product open V3
Samples can also be withdrawn from any of the sieve plates in the column by inserting
the syringe with the long, metal tip through the septum at the end of the appropriate glass spout
(see Figure 3). The septum heals when the syringe is withdrawn, preventing leakage. Handle the
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syringe with care because the column and the liquid samples are hot. Use a gas chromatograph
and the calibration curve in Figure H-1 to determine the ethanol/water mixture concentration.
Appendix E: Temperature Measurement
As shown in Figure 2, there are fourteen thermocouples located throughout the equipment,
designated as follows:
T1 = 1st (top) tray of distillation column
T2 = 2nd tray

T3 = 3rd tray

T4 = 4th tray

T5 = 5th tray

T6 = 6th tray

T7 = 7th tray

T8 = 8th tray

T9 = Temp of liquid in reboiler

T10 = Temp of vapor leaving the column above tray 1
T11 = Temp of cooling water entering condenser
T12 = Temp of cooling water leaving condenser
T13 = Temp of condensate and reflux/top product
T14 = Temp of feed liquid from feed tank
Temperatures may be viewed on the display on the right panel of the control console (Fig.
A-4). To display any temperature from T1 to T8, set the upper selector dial to the corresponding
station designation. To display temperatures T9 to T14, turn the upper selector dial fully
clockwise (to the furthest right setting) and then set the lower selector dial to the station
designation required. The distillation-unit software described in Appendix F enables real-time
visualization with a table and/or graph of any of the process temperatures. These data can also be
exported to Excel.
Appendix F: Distillation-Unit Software
Torunthesoftware,firstlogontothecomputer:
DIST 1
DIST 2
Username: CBE154
User
Password:
D1st1llat1on
D1st1llat1on
(Distillation with all letter i replaced by number 1)
Next, open the Distillation Column icon on the desktop. The initial screen will load
displaying a mimic diagram of the distillation unit shown in Figure F-1. The toolbar at the top of
the screen contains four buttons, which are used to navigate the software:
View Diagram displays a mimic diagram of the apparatus, with sensor readings
displayed in real time. Data values can be recorded by clicking the GO button.
View Graph displays a graph of selected recorded values.
View Table displays a table of recorded data.
View Presentation displays the presentation screens.
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Before operating the software, ensure that IFD: vCOM(3) m SE is displayed at the
bottom of the screen. If IFD: ERROR is displayed click red phone icon to start COM session,
select port COM3, and click OK. Also check the USB connection between the IFD5 and the PC
on the backside of the control console and confirm that the red and green LEDs are both
illuminated. Save your data using a USB flash drive.
Figure F-1 shows the Mimic Diagram, which gives a pictorial representation of the
equipment, with continuously updated display boxes for all the various sensor readings,
calculated variables etc. directly in engineering units. To view the Mimic Diagram click the View
Diagram icon from the main tool bar. Within the Graph and Table windows, you can record and
plot thermocouple and other process data at specified intervals. The data can later be exported to
Excel format for analysis.

Figure F-1: A screenshot of the Mimic Diagram of the distillation unit.

Appendix G: Feed-Pump Calibration

The peristaltic feed pump shown in Figure 2 delivers ethanol/water solution from the feed
tanks to one of the three feed points of the column. Adjustment of the the dial on the feed-pump
control console (illustrated in Figure A-3) controls the pump speed and, therefore, feed flow rate.
The dial has 10 full turns; each full turn is marked in one-hundredth segments. Figure G-1 shows
a calibration curve relating the feed flow rate [L/hr] to the dial reading on the feed-pump control
console for Pumps 1 and 2 corresponding to DIST1 and DIST2, respectively. The calibration was
produced by measuring the flow rate at 6-7 different dial readings between 0.5 and 3. Each point
shown is the average of triplicate measurements at each reading. Error bars indicating the range
of the three measurements are barely visible.

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Figure G-1: Volumetric feed flow rate [L/hr] versus dial reading for pumps 1 (red squares, red solid line)
and 2 (blue circles, blue dotted line), corresponding to DIST 1 and 2, respectively. The markers denote the
average of three measurements, and the error bars show the range, which is always <4% of the reading.
The lines are linear-regression best-fit lines; the fit equations appear in the legend at the top-left corner.

AppendixH:OperationoftheGasChromatograph
1.TheGCisalwaysinahotstandbymode(ifnot,asktheGSItoturniton).
2. Turn on the helium carrier pressure to 30 psi. The needle valve for the carrier gas is located
at the pressure regulator on the helium cylinder. Check that the green light for carrier gas is
on (on the front panel of the GC cabinet).
3. When carrier-gas flow is established, lift the red cover on the GC and flip the detector switch
to LOW current from its upright OFF position.

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FigureH1: Calibrationcurveforethanol/watermixturerelatingmolefractionofethanoltopeakarea
fractionofethanol.Eachpointistheaverageofthreemeasurements.ThelargestrangeofEtOHmole
fractionforeachpeakareafractionis0.003.

4. Turn on the computer attached to each GC unit using the following username and password:
Username:
Password:

Distillation
D1st1llat1on

5. Start the PEAK program from the icon on the desktop. Wait 30 min after initiation of PEAK
software before injecting first sample. Do not inject sample unless the temperature on the
front console of GC cabinet should read ~141 C.
6. Primeyourmicrolitersyringewiththesampletobetestedatleast35xbeforetestingeach
sample. This prevents cross contamination of the syringe between samples of different
composition.
7. Inject1Lofsampleusingthemicrolitersyringeinsertedintothesampleinjectionportand
clickthespacebaroricononthesoftwaretobeginthesampleanalysis.Zerothesensorby
clickingthe0icontotheleftofthegraph.
8. Onceseparateoutletpeaksareestablished,findtheareaunderthepeaksbyclickingView
Resultsfromthetopmenu,calculatetheethanolfractionalarea,andusethecalibration
curve/polynomialfitinFigureH1tofindacorrespondingethanolmolefraction.
9. Shut down the GC by turning the detector to the OFF position and exiting the PEAK
softwarecompletely.Closethevalvetotheheliumcylinder.
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