UNIVERSITI KUALA LUMPUR

MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING TECHNOLOGY

LABORATORY REPORT SUBMISSION FORM

To: AZYYATI BINTI JOHARI Subject: CKD 20102 SEPARATION TECHNOLOGY

From: (Student Name) Student ID No. Jotter Note (5 marks)

1. IMANI SUFIAH BT ZOLNIZAM 1. 55104118009
2. QAYSARRA NABELLA BT KAMISAN 2. 55104118007
3.AQIL IRFAN BIN MD.KHAIRULANWAR 3. 55104118036
4. MOHD KHAIRUL FATHY BIN M.ASRAR 4. 55102118037
5. 5.

Section: LO1-P1 Group No:3

Title of Experiment:
Packed Column Gas Absorption
Date of Experiment: Date of Submission:

` SUB TOPIC NOTE VERY POOR POOR MODERATE GOOD EXCELLENT

Brief review on the objectives of the experiment, main experimental results and significant discussion
Summary and conclusions obtained from the work 1 2 5 7 10

Introduction Theoretical of process and description of equipment (limited to 1 page only). 1 2 3 4 5

Objective List of objectives of experiment (rewrite the objectives listed). 1 2 3 4 5
Procedure Simplified procedure (start-up, analysis, experimental). Write in passive sentences. 1 2 5 7 10
Result/Data Tables of results, graph and calculation and sample calculation. 1 5 8 12 15
Discussion Graphical explanation (if any) and further discussion. 5 12 18 24 30
Conclusion Principal outcomes (related with objectives) and recommendation. (2 paragraphs only). 1 2 5 7 10
References At least three (5) references; book, manual, journal and internet sources. Write according to format. 1 2 3 4 5
Raw data during experiment (must be complete, tidy and signed) and any related diagram.
Appendix Jotter note (with signature). 1 2 3 4 5

TOTAL : 100 marks /100

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1.
Summary/ Abstract
0
*Write in this page only (1 page only).

Gas absorption is mass transfer operation where one or more species

is removed from a gaseous stream by dissolution in a liquid. Packed tower
with Rashchig Rings packings is used in the experiment. The main objective of
the experiment is to operate vapour–liquid separation experiment using a
Packed Column Gas Absorption Process Unit, analyze the sample using the
method of direct titration in order to determine the amount of NaOH reacted in
the mixture with the sample, calculate the concentration of CO 2 being
absorbed for every experimental time interval. The packed column is used to
flow the gas and liquid in a counter-current flow as it higher the efficiency of
absorption. The time of sample taken is increased each time by 10 minutes
until the 40th minute. And each of the sample differs in the content of CO2
concentration. The trend shown that the CO2 concentration lowers at each
time the sample taken. In this context, NaOH will showed less reaction if the
concentration increases, the reaction of NaOH mixture with the sample
decreases. As the flow rate of air increased, the absorption process also
increased. It is because the composition of the outlet volume of air increased
over time. Thus, all the objectives in this experiment is achieved. To deduce
the experiment, it is conducted successfully and all of the objectives are
achieved effectively.

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2.0 Introduction
*Write in this page only (1 page only). Any related diagram, put at Appendices.

In this experiment, the method implemented is separation by

gas absorption. In this context, the separation method is by gas-liquid
separation where the process involves the soluble parts of a mixture
are absorbed into a liquid [ CITATION Gea03 \l 17417 ]. The experiment
is conducted in a packed column/packed bed. The separation occurs to
the component of gas that is flowed at the liquid where the gas phase
will be absorbed into the liquid phase. In this experiment, the gas and
liquid streams are counter-currently run in the packed column. Every
single input of flow rates needs to be supervised wisely as a little error
can cause impact on the results in the end.

Packed column consists of three separated columns that is

denoted as C1, C2 and C3. The gas and liquid are counter-current
streamed so that the contact time is higher and absorption efficiency is
levered [ CITATION FUK77 \l 17417 ]. The packed column used
Raschig Rings as a medium. The gas that is CO2 will be feed from the
bottom inlet while the liquid will be feed from the top inlet. The flowrates
is controlled directly from the valve for each column. The water will be
circulated according to the time for the experiment .

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Objective

 Operate vapour–liquid separation experiment using a Packed

Column Gas Absorption Process Unit.
 Analyze the sample using the method of direct titration in order to
determine the amount of NaOH reacted in the mixture with the
sample.
 Calculate the concentration of CO2 being absorbed for every
experimental time interval.

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4.0 Procedure
*Write in 3 pages only.

Chemical preparation:
0.01 M HCl Standard Solution 1 litre
1. Withdraw 10 ml solution of HCl 1 M from the container.
2. Pour 10 ml solution of HCl 1 M into 1000 ml volumetric flask.
3. Add distilled water up to marked level at volumetric flask.
4. Shake the solution for a while.

0.01 M NaOH Standard Solution 1 litre

1. Weigh 0.4 g of 40 M NaOH pellets.
2. Pour NaOH pellets into 100 ml beaker.
3. Add distilled water into the 100 ml beaker.
4. Use magnetic stirrer to stir the mixture.
5. Pour the mixture into 1000 ml volumetric flask.
6. Add distilled water up to marked level at volumetric flask.
7. Shake the solution for a while.

Pre-start up checks:

1. Inspect the equipment visually for any damaged components or

glass breakage.
2. Ensure that the Cylindrical Re-circulation Vessel is charged with
water and that the liquid level is satisfactory (Refer to your
lecturer or technician).
3. Ensure valves FCV1, FCV2, FCV3, FCV4, V7, V12 and V13 are
closed.
4. Ensure valve V11 are open.
5. Choose the column to be operated (Ask lecturer/technician)
and adjust the following valves:

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Valve Column 1 Column 2 Column 3

Open Closed Open Closed Open Closed
V1 X X X
V2 X X X
V3 X X X
V4 X X X
V5 X X X
V6 X X X
V8 X X X
V9 X X X
V10 X X X
SV1 X X X

6. Ensure the manometer is reading zero.

7. Switch the selector valve SV1 to connect to the column chosen.

Setting up of Liquid Flow:

1.Check valves V11, V12 and FCV3 is closed and open valve V7.
2.Turn on the power switch of recirculation pump.
3.Slowly open valve FCV4 to give the required flowrate of 0.5 L/min as
indicated by FI3.
4.Ensure that the liquid overflow from the unit is connected to a suitable
drain.
5.Open valve V11 and V13 while close V7 when the water has entered
the column and when the flowrate has reached 1.5 L/min.
6.The unit is now ready to be used for experiment when the water has
come down from the column.

Experiment: Absorption of CO2 into water from Air-CO2 mixture

1. Open the water feed valve gradually until the desired flow rate
1.5 L/min is achieved as indicated in FI3. Ensure that the water
flow rate is allowed to stable for about 10 minutes after each
change until the desired value is reached.

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2. Open the Compressed Air Valve and ensure that the pressure is
1.5 bar gauge.
3. Depending on the column to be operated, OPEN the valve V1,
V2, or V3.
4. Gradually OPEN the feed valve FCV1 for Air flow until the
desired flow rate about 60 L/min is indicated in the flow meter
FI1. Allow flow rate of 40 L/min and increase to 60 L/min after
time elapse between 10 to 15 minutes. Ensure that you keep on
monitoring the Indicator from the manometer or DP1. Ensure
that there is no ‘sudden jump’ of the level. (Consult your lecturer
or technician). Ensure that the water flow rate is allowed to
stable for about 10 minutes after each change until the desired
value is reached.
5. After steady state conditions are reached, OPEN valve FCV2
GENTLY until CO2 rate is 2 L/min is achieved.
6. Allow further period of 10 minutes for the Absorption process to
attain steady state (Consult your lecturer or technician).
7. Draw at least 30 ml sample from the outlet valve, V12 for
every 10 minutes.

Direct Titration

1. Draw 10 ml of samples and pour into the 250 ml conical

flask. Add in 30 ml (V1) of prepared 0.01 M NaOH solution
(Consult your lecturer or technician concerning how to prepare
this solution). The volume of NaOH is in excess to ensure that

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all CO2 has reacted with NaOH in the mixture.

2. Add a few drops of an indicator (Phenolphthalein) to the
solution.
3. Pour in the already prepared 0.01 M HCl solution into the burette
and do titrate it with the mixture inside the conical flask.
4. Repeat the measurements every 10 minutes and carry out
the titration with FRESH samples until CONSTANT
concentration of NaOH has been achieved.
5. Record your results in Table 1.

General Shut-Down Procedure

1. Slowly close CO2 supply valve.

2. Slowly close the compressed air flow at FCV1.
3. Open V7.
4. Turn off the power switch of recirculation pump.
5. Turn off the air supply and CO2 supply (green valve).
6. Open V11 and allow fresh water to enter the column for a few
minutes to drain off the water.

5.0 Result/Data
*Tabulate/ Redraw the table consists of your result in this space. Attach graph paper (if any) or
sample calculation after this page.

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Time
(Minutes Volume Of HCl Titrated, V2 (mL) CO2 concentration
) (mol/Litre)
Averag
1 2 3 e
0
24 23 24 23.7 0.015
10
26 26 26 26.0 0.002
20
27 26 28 27.0 0.0015
30
28 27 29 28.0 0.001
40
28 28 29 28.3 0.001

6. Discussion
0
*Write in 2 pages only.

The purpose of the experiment was to Analyze the sample using the method
of direct titration in order to determine the amount of NaOH reacted in the
mixture with the sample, Calculate the concentration of CO2 being absorbed
for every experimental time interval and to Operate vapour–liquid separation
experiment using a Packed Column Gas Absorption Process Unit.
The theory of scheme is gas absorption is a process shich soluble
parts as a gas mixture are transferred to or dissolved In a liquid. The reverse
process called desorption , is used to transfer volatile parts from liquid
mixture togas A gas mixture travels up through a gas absorption tower in
standard packed column gas absorption, and the solution is transferred to
the liquid phase and thus gradually removed from the gas. On the way down
the column the liquid accumulates solute. The performance of a packed
colomns is very independent on the maitanance of good liquid and gas
distribution throughtout the packed bed and this is important consideration in
packed columns design. There were 2 type of absorption (physical and
chemical), depending whether is any chemical reaction between the solute
and solvent(absorbent).
The experiment was began with the preparation of 0.01M of HCl

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standard dilution and 0.01M NaOH standard dilution. 10ml of the 0.01M HCl
solution was withdraw then been added to volumetric flask that has 990ml of
distilled water, for the solution 0.4g naoh pallet was added into the
volumetric flask that contain of 90ml of distilled water and the solution was
stirred using magnetic stirrer. OPEN the Air flow valve FCV1 until the
desired flow rate approximately 60 L / min is indicated in the FI1 flow meter.
Allow 40 L / min flow rate, and increase to 60 L / min after 10 to 15 minutes.
Ensure that you continue to monitor the Manometer or DP1 indicator. Make
sure there is no Level 'sudden jump.' After it reached steady state conditions
are reached, OPEN valve FCV2 GENTLY until CO 2 rate is 2 L/min is
achieved. Allow further period of 10 minutes for the Absorption process to
attain steady state. For the direct titration, 10 ml of samples and pour into
the 250 ml conical flask. Add in 30 ml (V 1) of prepared 0.01 M NaOH
solution. Add a few drops of an indicator (Phenolphthalein) to the solution.
Pour in the already prepared 0.01 M HCl solution into the burette and do
titrate it with the mixture inside the conical flask. Repeat the measurements
every 10 minutes and carry out the titration with fresh samples until constant
concentration of NaOH has been achieved.
Based on the result recorded, the volume at minutes 0 for samples 1
was 24ml followed by samples 2 (23ml) and sample 3 (24ml). However,
when the times hit 10 minutes the volume for all three sample were constant
at (26ml). More over when 20minutes passed the volume for sample 1 was
(27ml), sample 2 was (26ml) and followed by sample 3 (28ml). At minutes 30
the volume increased for all sample, sample 1 (28ml), sample 2 (27ml) and
sample 3 (29ml). there is not much changes in minutes 40, where the
sample 1 and 2 constant at (28ml) also for sample 3 (29ml). when this data
been receive, average of all samples can be calculated. The average for
minutes 0 was (23.7ml), minutes 10 (26.0ml) and for minutes 40 (28.3ml).
Futhermore, CO 2 concentration also can be calculated were the

concentration of CO 2 at minutes 0 was the highest (0.015 mol/liter) and

decreased until minutes 40 (0.001 mol/liter).
There were few possible errors occur during the experiment, one of it
were the total drop of of an indicator (Phenolphthalein), a drop of it can
change all of the result. Secondly, the flowrate were not constantly at the
proper flowrate and its slightly change the data recorded. Last but not list,
time for take the data must be well prepare of it can totally change the result.

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7. Conclusion
0

In conclusion, based on the results obtained from the experiment

shows that when the concentration increase, the volume of titrated
HCl decreases. The experiment where to analyze the sample using
the method of direct titration in order to determine the amount of
NaOH reacted in the mixture with the sample. In this experiment, as
NaOH solution enters from the top and the mixture of air enters at the
bottom of the column. NaOH will showed less reaction if the
concentration increases, the reaction of NaOH mixture with the
sample decreases. As the flow rate of air increased, the absorption
process also increased. It is because the composition of the outlet
volume of air increased over time. Thus, all the objectives in this
experiment is achieved.

Some suggestion in improving the safety are to always check

and rectify any leak and all operating instructions supplied with the
unit must be carefully read and understood before attempting to

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operate. Next, be extremely careful when handling hazardous,

flammable or polluting materials such as CO₂. Make sure the system
is sufficiently ventilated when working at atmospheric pressure.

8. Reference(s)
0

References
FUKUSHIMA, S. &. (1977). Interfacial area and boundary of hydrodynamic
flow region in packed column with cocurrent downward flow.
Journal of Chemical Engineering of Japan,, 461-467.
Geankoplis, C. J. (2003). Transport processes and separation process
principles:(includes unit operations). Prentice Hall Professional
Technical Reference.
iitb.vlab.co.in. (2011). Gas Liquid Absorption. Retrieved from Sakshat
VirtualLabs: http://iitb.vlab.co.in/?
sub=8&brch=116&sim=951&cnt=1
McCabe, W. S. (1993). McCabe, W., Smith, J., & Harriott, P. McGraw-Hill
Book Co.
R.H. Perry, C. H. (1973). Chemical Engineers' Handbook. In C. H. R.H.
Perry, Chemical Engineers' Handbook. New York:McGraw-Hill
Book Company.

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9. Appendices
0
*Put raw data, signed jotter note and related diagram in this section.

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