FACULTY OF CHEMCIAL ENGINEERING UITM PASIR GUDANG

CHE 246 SEPARATION

PROCESS
LAB INSTRUCTION
A. DISTILLATION COLUMN
B. GAS ABSORPTION

CHE 246

DEC-APR15

SECTION 1: DISTILLATION COLUMN

NOTES OF GUIDANCE
Lab work
Activity 1 Continuous distillation at constant reflux.
Learning outcome
1. Describe the operation of continuous distillation column.
2. Draw the PFD and P&ID of continuous distillation column.
3. Perform mass balance calculations on continuous distillation column.
4. Demonstrate effective team role and responsibility in the task execution.
Scenario
You have just joined as an assistant engineer in Maju Jaya Pte Ltd which produces methanol. The
process engineer asks you and your team to operate a continuous distillation column at constant reflux
ratio. In addition, you have to carry out mass balance calculations on the distillation column and
examine the effects of reflux ratio and feed conditions on the number of theoretical plates in a
continuous distillation. Refer to information of distillation column.
Objectives
This activity requires you to operate a continuous distillation column at constant reflux, carry out mass
balance calculations on the distillation column and examine the effects of reflux ratio and feed
conditions on the number of theoretical plates in a continuous distillation.
The process engineer has provided you the following information;
1. Schematic diagram of the distillation unit (Appendix: Figure 1)
2. X-Y Equilibrium Diagram for Methanol-Water System at 1 atm (Appendix: Figure 2)
Upon completion of the test, write a technical memo of the result obtained. The memo should include
(but not limited to) the following
a) Clearly states test parameters
b) Test results
c) Evaluation of results
Pre-Experiment Assessment
A. Planning/Preparation (10 marks)
All team members arrive at the process operation site to discuss on the plan to examine the effects of
reflux ratio and feed conditions on the number of theoretical plates in a continuous distillation. Please
record as the team members in the process operation site by video.
Task
I.
Distributed works and introduces the team.
II.
Familiarize with the distillation column by determining the line tracing of this system.
reference to Figure 1, identify the key components of the distillation column.

@R

With

Page 1

CHE 246

DEC-APR15

2. Understand how the distillation column works

a. The function of column, reflux drum, condenser and reboiler in distillation column.
b. Explain distillation principles; volatility prior to boiling point of the component
3. Decide on the test parameters
a. Reflux ratio and feed temperature
B. Allocation of Roles and Teamwork (10 marks)
1. Analyze the tasks to be performed and divide among your team who to perform the tasks.
No
1
2
3
4
5

Task description
Introduction and theory
Collecting data
Analyze the result
Safety awareness
(Add if necessary)

Member

2. Explain the basis for your groups task allocation.

3. Explain how will failure in performing the role of one of the above mentioned task affect the team
performance.
C. Hazard Identification and Safety Precaution (10 marks)
Before starting the operation of the distillation column, it is important to identify hazards and precautions
to be taken to ensure safety of operators.
Study the process equipment, utilities involved, process materials and procedures carefully to identify
potential hazards.
1. What are the hazards associated with ethanol?
2. What are the possible hazards if ethanol-water mixture is exchange to benzene-toluene mixture in
the process operation?
3. What safety precautions would you take in relation to the above mentioned hazards?
D. Performance Test Procedure
1. Perform the general start-up procedures.
a) Ensure all valves are closed.
b) Turn on the power for the control panel.
c) Prepare a 3040 L mixture containing ethanol and filtered water at the desired composition.
Charge the unit as follows:
i. Open the charge port cap at the reboiler B1, and fill the reboiler up to the level of the internal
overflow height.
ii. Pour the remaining ethanol-water mixture into the feed vessel B2 through the feed charge port.
d) Set the reflux divider KFS-101 to total reflux. This is to prevent any distillate from escaping when
starting up the distillation column.
@R

Page 2

CHE 246

DEC-APR15

e) Let the cooling water flow into the condenser W2 and product coolers W3 & W4 by opening valves
V13, V14 and V15.
f) Ensure that the tip of the level switch is located below the reboiler equator, which is at the liquid
inlet from the cartridge heaters.
g) Switch on the cartridge heaters at W1. Allow the liquid in the reboiler to boil.
h) Observe the vapor rising from the boiling liquid into the distillation column. As the vapor reaches
the condenser, it will condense and flow back into the column as liquid. Mass transfer will take place
between this liquid and vapor phase in the column.
i) Check that the condenser has sufficient cooling water flow to minimize escape of vapor into the
vent.
j) Let the distillation column run until a stable condition is observed. The stable condition is reached
when all temperature indicators on the column give a constant reading with an allowable fluctuation
of 0.2C.
2. Set the reflux divider to automatic reflux with a reflux ratio of 1 (e.g. 2 sec reflux and 2 sec distillate)
at the reflux divider controller (KFS-101).
4. Switch on the feed pump P1 and adjust the pump stroke and frequency in order to obtain a flow rate
between 5 to 10 L/hr (80 to 100% stroke at 120 to 150 strokes/minute).
5. Switch on the bottom pump P2 and adjust the bottom flow rate (V7) to desired value by taking into
account of the feed and distillate flow rate to maintain the level in the reboiler.
6. Once the distillation column has reached stable condition, record the trays, top and bottom
temperature.
7. Collect samples from the trays, distillate and bottom product. Samples can be taken from the
distillate and the bottom product for analysis:
a. Distillate sampling:
i) Drain any remaining liquid in the sampling valve V11.
ii) Place a vial below valve V11.
iii) Set the reflux divider to total distillate offtake for a few seconds.
iv) Open valve V11, collect enough sample and close the valve.
v) Switch the reflux divider back to the original setting.
b. Bottom sampling:
i) Drain any stagnated liquid above valve V8.
ii) Place a vial below valve V8.
iii) Open valve V8, collect enough sample and close the valve. Be careful of the hot liquid while
collecting a sample.
iv) Cool the sample by immersing the vial in cold water.
Note: Always re-cap the vials quickly after collecting samples to avoid excessive evaporation of
ethanol before analysis.
8. Measure the refractive index for all samples and determine their compositions.
Measure the refractive index of a sample and determine its composition from the calibration curve. If
the composition value is difficult to be determined accurately due to the calibration curves flat slope,
dilute the sample so that a more accurate reading can be obtained. Perform the dilution as follows:
a. Place a 10 mL measuring cylinder on a weighing scale (accurate to 0.01 g) and zero the scale.
@R

Page 3

CHE 246

DEC-APR15

b. Using a dropper, transfer 1 to 2 g of sample into the measuring cylinder. Record the sample
weight.
c. Add water into the measuring cylinder to dilute the sample. Obtain a total solution weight in the
range of 5 to 10 g. Record the solution weight.
d. Ensure that the diluted solution is well mixed before measuring its refractive index (RI).
e. Obtain the diluted solution's composition from the calibration curve.
f. Calculate the actual sample's composition.
g. Use the sample table in Appendix C for data recording and calculation
9. Measure the bottom and distillate product flow rates at FI-302 and FI-303.
10. Repeat the experiment (steps 3 to 8) with a different value of reflux ratio.
11. Repeat the experiment (steps 4 to 8) with a different feed temperature by switching on the feed
preheater W5 and setting the feed temperature set point to 50C.
E. Post-Experiment Assessment (10 marks)
You have completed the task. Carry out a team review on the test result.
1. Draw the PFD and P&ID of distillation column.
2. Write down the overall and component material balance equations for the distillation column.
3. Identify at least 2 observations (flaws or good features) made during the operation on the basic
function of the distillation column.
REPORT ASSESSMENT (10 MARKS)
F. Technical Memo
Draft a technical memo addressed to the Process Engineer on your teams evaluation of the distillation
unit. Your memo can take the technical format report.
Enclosed: Test results of distillation column at constant reflux ratio and key findings
The enclosed Test results of distillation column at constant reflux ratio and key findings of the memo
should include detailed test results and key findings as follows:
a) Test results. State the test parameters and provide proper tabulation with units clearly stated.
b) Evaluation of results.
For the section on Evaluation of results, you may use the following guiding questions to discuss the
results:
By using X-Y equilibrium diagram for ethanol-water system
1. Mark the trays, top and bottom compositions on the diagram
2. Determine the number of theoretical plates in the distillation column using the McCabe-Thiele
method.

@R

Page 4

CHE 246

DEC-APR15

SECTION 2: GAS ABSORPTION

NOTES OF GUIDANCE
Lab work
Activity 2: Gas Absorption.
Learning outcome
1. Describe the operation of gas absorption column.
2. Draw the process flow diagram (PFD) and piping and instrumentation diagram (P&ID) of gas
absorption column.
3. Demonstrate effective team role and responsibility in the task execution.
Scenario
You have just joined as an assistant engineer in Linde Pte Ltd. You and your teammates have given a
task to operate a gas absorption column of a carbon dioxide (CO2) with water as solvent. In addition,
you have to calculate the rate of absorption of CO2 into water. You can refer any references related to
the theory.
Objectives
This activity requires you to operate gas absorption column, carry out mass balance calculations on the
gas absorption column and examine the effects of flow rate of CO2 into water.
Upon completion of the test, write a technical memo of the result obtained. The memo should include
(but not limited to) the following:
a) Clearly states test parameters
b) Test results
c) Evaluation of results

@R

Page 5

CHE 246

DEC-APR15

A. Planning/Preparation (10 marks)

All team members arrive at the process operation site to discuss on the plan to examine the effect of
CO2 absorption rate into water.
1. Familiarize with the gas absorption column by determining the line tracing of this system.
2. Understand how the gas absorption works
a) The function of each component in the gas absorption column (receiving vessels, absorption
column, centrifugal pump).
b) Explain gas absorption principles.
3. Decide on the test parameters
B. Allocation of Roles and Teamwork (10 marks)
Analyze the tasks to be performed and divide among your team who to perform the tasks.
no
1
2
3
4
5

Task description
Introduction and theory
Collecting Data
Analyze the result
Safety awareness
(any if necessary)

Member

Explain the basis for your groups task allocation.

Explain how will failure in performing the role of one of the above mentioned task affect the team
performance.
C.

Hazard Identification and Safety Precaution (10 marks)

Before starting the operation of the gas absorption column, it is important to identify hazards and
precautions to be taken to ensure safety of operators. Study the process equipment, utilities involved,
process materials and procedures carefully to identify potential hazards.
1. What are the hazards associated with the operation of gas absorption column?
2. What safety precautions would you take in relation to the above mentioned hazards?
D.

Performance Test Procedure

1.0
1.1

OPERATING PROCEDURES
General Operating Procedures
It is important that the user read and fully understand all the instructions and precautions stated
in the manufacturer's manuals supplied with the absorption unit prior to operation. The following
procedures will serve as a quick reference for operating the unit.

1.2

General Start-Up Procedures

a) Ensure all valves are closed except the ventilation valve V13.
b) Check that all gas connections are properly fitted.
c) Open the valve on the compressed air supply line. Set the supply pressure to between 2 to 3
bar by turning the regulator knob clockwise.

@R

Page 6

CHE 246

DEC-APR15

d) Open the shut-off valve on the CO2 gas cylinder. Check that the CO2 cylinder pressure is
sufficient. Replace the cylinder if necessary.
e) Turn on the power for the control panel.
1.3

General Shut-Down Procedures

a) Switch off pump P1.
b) Close valves V1, V2 and V12.
c) Close the valve on the compressed air supply line and exhaust the supply pressure by
turning the regulator knob counterclockwise all the way.
d) Close the shut-off valve on the CO2 gas cylinder.
e) Drain all liquid in the column K1 by opening valve V4 and V5.
f) Drain all liquid from the receiving vessels B1 and B2 by opening valves V7 and V8.
g) Drain all liquid from the pump P1 by opening valve V10.
h) Turn off the power for the control panel.

1.4

Liquid Sampling Procedures

Samples can be taken from the liquid entering and exiting the absorption column for analysis.
The sampling valves are located at:
a) V8 for inlet liquid to absorption column K1
b) V7 for outlet liquid from absorption column K1
The procedures for collecting a sample are as follows:
a) Drain any stagnated liquid above the sampling valve.
b) ii) Place a vial below the sampling valve.
c) iii) Open sampling valve and collect about 100 mL of sample.
d) iv) Close the sampling valve.

1.5

Analysis of Dissolved CO2 in Water

Water used for absorption should be deionised because presence of dissolved salts could affect
the analysis method as described below.
CHEMICALS NEEDED:
a) Deionised and CO2 free water
b) Phenolphthalein indicator (AR grade)
c) 1.0 L of standard 0.05 M sodium hydroxide (NaOH) solution
d) 100 mL of standard 0.01M sodium bicarbonate (NaHCO3) solution
PROCEDURES:
a) Obtain a sample from Section 4.4.
b) Prepare exactly 100 mL of sample in a conical flask.
c) Add 510 drops of phenolphthalein indicator. If the sample turns red immediately, no free
CO2 is present. If the sample remains colourless, titrate with the standard 0.05 M NaOH
solution.
d) Measure the volume of 0.05 M NaOH required to reach the end point. The end point
occurs when a definite pink colour persists in the solution for longer than 30 seconds.
e) For best results, use a colour comparison standard. Prepare exactly 100 mL of 0.01 M
NaHCO3 solution in a conical flask and add 510 drops of phenolphthalein indicator.

@R

Page 7

CHE 246

2.0

DEC-APR15

EXPERIMENTAL PROCEDURES:
a) Fill the receiving vessel B2 through the charge port with 25 L of deionised water by opening
valve V3 and V5.
b) Close valve V3.
c) Open valve V10 and valve V9 slightly. Observe the flow of water from vessel B1 through
pump P1.
d) Open and adjust valve V1 to give a flow rate of 30 L/min air into column K1.
e) Open and adjust valve V2 to give a flow rate of 2 L/min CO2 into column K1.
f) For continuous monitoring of CO2 composition at the outlet gas flow, open valve V12 and
slowly close valve V13 to give a flow rate of 2 L/min at FT-304. Always maintain this flow
rate throughout the experiment.
g) Monitor the CO2 composition at QI-401 until it is constant. Record the value.
h) Switch on pump P1, then slowly open and adjust valve V11 to give a water flow rate of
around 0.5 L/min. Allow the water to enter the top of column K1, flow down the column and
accumulate at the bottom until it overflows back into vessel B2.
i) Start collecting liquid samples from both inlet and outlet of absorption column K1 (Section
4.4). Always collect the samples simultaneously.
j) To collect liquid sample for outlet of the adsorption column, close valve V5, open valve V4
and V7.
k) After finish collecting sample, close valve V4 and V7, open valve V5.
l) Analyse the collected samples to determine the composition of dissolved CO2 (Section 4.5).
m) At the same time, record the outlet CO2 composition at QI-401.
n) Continue to collect the liquid samples and record the outlet CO2 composition at every 5minute intervals until there are no more changes in CO2 composition over time.
o) Throughout the experiment, monitor and maintain the air, CO2 and water flow rates by
adjusting the appropriate valves.
p) At the end of the experiment, close valves V1, V2 and V12. Switch off pump P1. Transfer all
the CO2 rich water in receiving vessel B1 to vessel B2.
q) Repeat the experiment (steps 2 to 14) by changing the water flow rate from 0.5 to 1 L/min.
r) Perform shut down procedure

E.

@R

Post-Experiment Assessment (10 marks)

a) Use the sample table in Appendix A, B, for data collection.
b) Plot the CO2 concentration in the outlet water flow as a function of time.
c) Plot the CO2 concentration in the outlet gas flow as a function of time.
d) Compare the CO2 concentration plots for different water flow rates.

Page 8

CHE 246

DEC-APR15

REPORT ASSESSMENT (10 MARKS)

F. Technical Memo
Draft a technical memo addressed to the Process Engineer of Linde Pte Ltd. on your teams evaluation
of the distillation unit. Your memo can take the format of technical report format.
Enclosed: Test results of gas absorption and key findings
The enclosed Test results of gas absorption rate and key findings of the memo should include detailed
test results and key findings as follows:
a) Test results. State the test parameters and provide proper tabulation with units clearly stated.
b) Evaluation of results.
For the section on Evaluation of results, you may use the following guiding questions to discuss the
results:
a) Calculate the concentration of CO 2.
(Sample calculation of Concentration of CO 2 in Feed Tank)
Let say volume of NaOH needed to reach end point = y ml,
Molarity of NaOH = 0.05 mol/L,
Thus, concentration of CO2 in Feed Tank = (mol/l).
b)
c)
d)
e)

@R

Plot the graph CO2 concentration in the outlet water flow as a function of time.
Plot the CO2 concentration in the outlet gas flow as a function of time.
Compare the CO2 concentration plots for different water flow rates.
Calculate the rate of absorption into water.

Page 9

CHE 246

DEC-APR15

APPENDICES

@R

Page 10

CHE 246

DEC-APR15

APPENDIX A
Theory on Distillation Column
The principle for continuous distillation is the same as for normal distillation: when a liquid mixture is
heat so that it boils, the composition of the vapor above the liquid differs from the liquid composition. If
this vapor is then separated and condensed into a liquid, it becomes richer in the lower boiling
component(s) of the original mixture. This is what happens in a continuous distillation column. A mixture
is heated up, and routed into the distillation column. On entering the column, the feed starts flowing
down but part of it, richer in lower boiling component(s), vaporizes and rises. However, as it rises, it
cools and while part of it continues up as vapor, some of it (enriched in the less volatile component)
begins to descend again. Since a continuous distillation unit is fed constantly with a feed mixture and
not filled all at once like e a batch distillation, a continuous distillation unit does not need a sizable
distillation pot, vessel, or reservoir for a batch fill. Instead, the mixture can be fed directly into the
column, where the actual separation occurs. The height of the feed point along the column can vary on
the situation and is designed so as to provide optimal results. A continuous distillation is often a
fractional distillation and can be a vacuum distillation or a steam distillation.

Figure 1: A binary distillation separates a feed mixture stream into two fractions: one distillate and one
bottoms fractions
@R

Page 11

CHE 246

DEC-APR15

SAMPLE TABLE FOR PREPARATION OF CALIBRATION CURVE

Purity of ethanol = __________
Density of ethanol = _____ g/mL
Density of water = _____ g/mL
Molar volume of ethanol = _____ mol/mL
Molar volume of water = _____ mol/ml

@R

Page 12

CHE 246

DEC-APR15

SAMPLE TABLE FOR EXPERIMENTS 1

Initial reboiler composition=
Feed temperature =
Reflux ratio = _____
Feed flow rate = _____ LPM
Distillate flow rate = _____ LPM
Bottom product flow rate = _____ LPM

@R

Page 13

CHE 246

DEC-APR15

PHYSICAL PROPERTIES OF COMPONENTS

Properties of Pure Components

@R

Page 14

CHE 246

DEC-APR15

Figure: 2 X-Y Equilibrium Diagram for Methaol-Water System at 1 atm

@R

Page 15

CHE 246

DEC-APR15

APPENDIX B
Theory on Gas Absorption
Gas absorption is a unit operation in which soluble components of a gas mixture are dissolved into a
liquid phase. Absorption, in common with distillation, makes use of special equipment for bringing gas
and liquid phases into intimate contact. Gas absorption is a unit operation in which soluble components
of a gas mixture are dissolved into a liquid phase.
It is meant to demonstrate the absorption of carbon dioxide into water in a packed column. The gas and
liquid normally flow counter currently, and the packings serve to provide the contacting and
development of interfacial surface through which mass transfer takes place.
Consider a system in which a gaseous component A is in equilibrium with both air and water at a given
temperature. The equilibrium relationship between the partial pressure, pA in the gas phase and the
composition, xA in the liquid phase can often be expressed by a straight line Henrys Law equation at
low concentrations.
pA = H xA

[1]

where H is the Henrys Law constant for the given system expressed in atm/mole fraction. If both sides
of the equation is divided by the total pressure, P in atm, the composition, yA in the gas phase can be
related below:
yA = H xA

[2]

where H is equal to H/P. However, H is more often used because it is independent of the total system
pressure. Equilibrium data for most systems follow Henrys Law up to a concentration of about 1 mol%
in the liquid phase.

Single stage equilibrium process.

One in which two different phases are brought into intimate contact with each other and then are
separated. Various components transfer between the two phases and are essentially at equilibrium with
each other after considerable mixing. The process can be represented in Figure 2 below.

@R

Page 16

CHE 246

DEC-APR15

Figure 3: Gas absorption column.

@R

Page 17

CHE 246

DEC-APR15

SAMPLE TABLE FOR EXPERIMENT 2

Process: Absorption
Air flow rate :
CO2 flow rate :
CO2 inlet composition :
Liquid flow rate :

Time (min)

L/min
L/min
vol%
L/min
Outlet gas
Vol% of CO2 in outlet
gas

Outlet water
Vol% of NaOH for
Vol% of CO2 in outlet
sample titration (mL)
water

0
5
10
15
20
25
30
35
40
45
50
55
60

@R

Page 18

CHE 246

DEC-APR15

APPENDIX C
Assessment
This activity contributes 20% of the marks weighting for this course. The distribution of marks for the
various activity component is contain in Table 1
Criteria
Lab
Preparation

1
Unprepared
and needs
complete
directives from
demonstrator

2
Marginal
preparation,
needs
constant
supervision

3
Prepreparation is
satisfactory.
Requires
occasional
reminders.

Following
Procedure

Lacks the
appropriate
knowledge of
the lab
procedures

Demonstrates
general
knowledge of
lab
procedures

Demonstrates
good
knowledge of
the lab
procedures

Often requires
help from the
demomstrator
to even
complete
basic
procedures

Requires help
from
demonstrator
with some
steps in
procedures

Asks peers for

help with
problems in
lab
procedures

Measurements
are
incomplete,
inaccurate and
imprecise

Measurements
are somewhat
inaccurate and
very imprecise

Data
Collection

Observations
are incomplete
or not included
Symbols, units
and significant
figures are not
included

@R

Works to
follow each
step before
moving on to
the next step

Observations
are incomplete
or recorded in
a confusing
way
There are 3 or
more minor
errors using
symbols, units
and significant
digits or 2
major errors

Measurements
are mostly
accurate
Observations
are generally
complete
Work is
organized
Only 2 or 3
minor errors
using symbols,
units and
significant
digits

4
Prepreparation is
very good.
Seems to
know
everything that
is required.
Demonstrates
sound
knowledge of
lab
procedures

5
Prepreparation is
excellent. Will
often help
others in the
experiments.

Discuss with
peers to solve
problems in
procedures

Gladly helps
other students
to follow
procedures

Carefully
follows each
step

Thoroughly
and carefully
follows each
step before
moving on to
next step

Measurements
are accurate
with
reasonable
precision

Measurements
are both
accurate and
precise

Observations
are thorough
Work is
generally neat
and
organized.
Includes
symbols, units
and significant
digits

Points

Demonstrates
very good
knowledge of
the lab
procedures

Observations
are very
thorough and
may recognize
possible errors
in data
collection
Work is neat
and
organized.
Includes
appropriate
symbols, units
and significant
digits

Page 19

CHE 246

Safety

DEC-APR15

Proper safety
precautions
are
consistently
missed
Needs to be
reminded
often during
the lab

Proper safety
precautions
are often
missed

Proper safety
precautions
are generally
used

Needs to be
reminded
more than
once during
the lab

May need to
be reminded
once during
the lab

Proper safety
procedures
are
consistently
used

Proper safety
precautions
are
consistently
used

Uses general
reminders of
safe practices
independently

Consistently
thinks ahead
to ensure
safety
Will often help
other students
to conduct
labs safely

Q&A
Session

Very poor
responses to
questions.

Marginal
responses.
Needs
guideline to
the correct
answers.

Satisfactory
responses to
questions with
occasional
mistakes

Very good
responses to
questions and
exhibit above
average
knowledge on
experiments

Exhibit
excellent
responses to
questions and
able to discuss
the subject
matter

Clean-up

Proper cleanup procedures

are seldom
used

Needs to be
reminded
more than
once during
the lab to use
proper cleanup procedures

Proper cleanup procedures

generally used

Consistently
uses proper
clean-up
procedures

Consistently
uses proper
clean-up
procedures

help to
complete
clean-up

1 or 2 items
left at station
or not cleaned

Station
generally neat
and clean

Often will help

other students
to complete
tasks properly

3 or more
items left at
station or
station not
cleaned
Unacceptable

Station
generally left
clean

May need
some help on
occasion to
complete
tasks
Station always
left neat and
clean

Station
generally left
clean

Marginal

Acceptable

3 or more
items left at
station or
station not
cleaned
Exceptional

Overall
performance

@R

Excellent

Page 20