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7.1 DESCRIPTION
7.1.1 Introduction
2
9 19
17
10 18
11
12 13 22 21 14 15 20 16
2. TU-U: ‘U’ shaped tube with two glass spheres where the solution with which
the CO2 of a sample taken with the syringe (JE) will be retained is introduced.
4. VT-1: ‘T’ valve used to communicate line B and/or the syringe (JE) with the
atmosphere.
5. VT-2: ‘T’ valve used to communicate line B with line C and/or the U shaped
tube (TU-U).
6. VT-3: ‘T’ valve used to open or close the left hand branch of the M-1 and/or
M-2 manometer with the upper or middle point of the column (COL).
7. VT-4: ‘T’ valve used to open or close the right hand branch of the M-1 and/or
M-2 manometer with the upper or middle point of the column (COL).
8. VT-5: ‘T’ valve used to communicate line C with the upper or middle point of
the column (COL) to take samples.
9. M-1: U shaped manometer to measure the pressure drop of the column bed
(COL) between the upper and lower point or middle and lower point.
10.M-2: U shaped manometer to measure the pressure drop of the column bed
(COL) between the upper and lower point or middle and lower point.
11.V-6: Valve that opens or closes the lower part of the U shaped tube (TU-U),
12.V-7: Valve that opens or closes the lower part of the manometer (M-1), which
is the area where the liquid used to measure pressure differences (H2O in our
case) is introduced or removed.
13.V-8: Valve that opens or closes the lower part of the manometer (M-2), which
is the area where the liquid used to measure pressure differences is introduced
or removed.
14.VR-1: Valve that regulates the air flow that enters through the compressor
(ACO-1).
15.VR-2: Valve that regulates the CO2 flow that enters through the cylinder that
introduces that gas.
16.VR-3: Valve that regulates the water flow that enters through the water pump
AB-1.
17.C-1: Flowmeter to indicate the air entering the lower part of the column (COL).
18.C-2: Flowmeter to indicate the flow of CO2 entering the lower part of the
column (COL).
19.C-3: Flowmeter to indicate the flow of water entering the upper part of the
column (COL).
21.V-10: Valve to open or close the measuring line of the CO2 meter for a
22. V-11: Valve to open or close the measuring line of the CO2 meter for a
sample that correspond to the middle or upper part of the column COL.
This valve is optional in the CAG unit.
6 1
1. V-9: Valve used to take samples of the water that reaches the lower part of the
column (COL).
4. AB-1: Pump to supply the inlet water from the tank (TAA).
5. SC-3: Sensor to measure the inlet flow of water at the upper part of the column
(COL). *Available in the CAGC unit.
6. VR-4: Valve that regulates the water flow that leaves through the lower part of
the column (COL) towards the tank (TAA).
Liquid circuit
The liquid, stored in a tank (TAA) made of PVC, is driven to the column
with the aid of a magnetic drive centrifugal pump. The water flow that reaches the
column is measured with a flowmeter (C-3) or with the flow sensor (SC-3) (if the unit
is the CAGC version) and it is regulated with the valve (VR-3) and/or through the
software actuator (if the unit is the CAGC version).
The liquid is supplied to the column (COL) through its head with a glass
diffuser. After crossing the column (COL), water passes to the storage tank (TAA)
through a pipe with a hydraulic sealing to prevent leakages. There is a flow regulation
valve (VR-4) and a sample taking valve (V-9).
Gases circuit
Both gaseous currents are mixed and then introduced at the base of the
column (COL) through a lateral inlet located below the bed level, so that the gaseous
mixture is as homogeneous as possible. The air and CO2 will be expelled through the
upper side of the column (COL) towards the atmosphere. For that reason, good
ventilation is needed in the surroundings of the gas outlet.
When starting the liquid circuit and gases circuit at the same time, after a
while, water will have absorbed a certain amount of CO2 and the rest will be expelled
to the atmosphere. Samples can be taken to be analyzed with solutions that allow to
absorb the CO2, as the KOH solution.
- Two manometric tubes (M-1 and M-2) to determine the pressure drop
in the column.
It consists of:
• CO2 digital meter with reading via software. The CO2 concentration in the currents
coming from the upper and lower parts of the column can be directly measured. This
meter is optional for the CAG unit.
- COL: the column is a cylindrical tube made of glass with a length of 1400
mm and inner diameter of 75 mm.
- SC-1: Sensor to measure the air flow. o Operating range: 5.2-80 l/min.
o KOH solute.
to collect effluents.
One of the factors that influences when designing the diameter of a packed
column is the flow rate of fluids, gas and liquid, that turns out to be tolerable through the
packed bed.
D'
D
C' Bubblers Area
C
Point of Flooding
B'
Load Area
B
Load or Drag Point
A'
Dry
Filling
Figure 2 – Pressure drop of the gas through the packing: drag and flooding velocities
From point B on, when increasing the gas volume, (no matter the volume
of liquid taken into account) the pressure drop starts being proportional to a power of
the gas velocity higher than 2 and increasing continuously. Point B is the load or drag
point, defined by a velocity of the gas and load or drag gas volume.
When increasing the flow of gas above the load or drag value, a point in
the curve is reached (C) in which it tends to be vertical. At that moment the liquid
retention in the packing increases so much that it stops flowing down and all the gaps
between packing pieces are filled with liquid. The gas bubbles in the core of the liquid,
increasing its pressure drop extraordinarily. Point C is the flooding point. The gas
velocity and flow that correspond to this point are called flooding velocity and flooding
flow rate. The flooding phenomenon is demonstrated in the column by the
accumulation or retrogression of the liquid inside, since the pressure drop in the gas is
so high that the load of liquid is not enough to flow against that pressure.
The inlet and outlet flows of liquid (L) and gaseous mixture (G) are constant along
a packed column. Therefore, the overall mass balance can be expressed as:
Where,
(dimensionless)
Mole fraction of CO2 in the mixture (air + CO2) at the inlet of
the column.
(dimensionless)
Mole fraction of CO2 in the mixture (air + CO2) at the outlet
of the column.
(dimensionless)
Mole fraction of CO2 in the water at the inlet of the column. It
is practically non-existent, water does not contain CO2.
Mole fraction of CO2 in the water at the outlet of the column. (dimensionless)
Subscripts 1 and 2 are used to designate the currents at the inlet and outlet
of the column respectively.
Generally, the hypotheses below are taken into account in order to study
the mass balance of a continuous and stationary absorption process in a packed column
theoretically:
- Only one solute is transferred from the gaseous state to the liquid state.
- Both phases flow in countercurrent (the liquid descends and the gas
ascends).
- It is supposed that the pressure drop of the gas when crossing the column
is negligible compared to the total pressure and that the balance is
established in the interface instantaneously, that is to say, it does not offer
resistance to the mass transfer.
Nevertheless, the height of the column and, therefore, the total volume of
packing, depend on:
Thus, height calculations are based on mass and energy scales balances and
on the estimate of the driving forces and individual mass transfer coefficients during
the liquid and gaseous phases (kl and kg). If the resistance of one of the two phases
controls the transfer process, it will only be necessary to know the individual mass
transfer coefficient through that phase, since it will practically coincide with the overall
coefficient.
It can be demonstrated that the overall mass transfer coefficient through the
liquid phase is obtained by this formula:
Where:
Before starting the practical exercises, it is essential to know how to perform the
operations described below:
a. Check that the air regulation valve (VR-1) is open and that the CO2 cylinder
regulation valve (VR-2) is closed.
c. Fix the desired value for the air flow with the valve (VR-1) and record the value of
the flow using the flow meter (C-1) or from the value indicated by the sensor (SC-
1) if the unit is the computerized version.
*In the CAGC unit the volumetric flow is indicated by the sensor (SC-
1).
e. To calculate the mass flow under standard conditions (1 bar and 25ºC):
e. Regulate the air flow and the CO2 flow with the regulation valves (VR-1 and VR-
2).
f. Record the value indicated by the flow meters (C-1 and C-2) or from the value
indicated by the sensors (SC-1 and SC-2) if the unit is the computerized version.
Please note that as the air and the CO2 are connected in the same conduit,
regulating one of the flows influences the other flow. For that reason they
must be regulated when both gases are flowing.
*In the CAGC unit, the volumetric flow is indicated by the sensors
h. To calculate the mass flow rates under standard conditions (1 bar and 25ºC):
a. Check that the water flow regulation valve (VR-3) and the water flow outlet
regulation valve (VR-4) are fully open to allow water run freely.
c. Fix the desired value for the water flow with the valve (VR-3). It can also be
d. Record the flow value using the flow meter (C-3) or from the value indicated by
the sensor (SC-3) if the unit is the computerized version.
As it can be observed the unit has two manometers (M-1 and M-2) to
measure the pressure drop inside the column (COL). In the CAGC unit, apart from
these manometers, there are pressure sensors (SPD-1 and SPD-2) that indicate the
pressure along the column directly (COL).
Valves must be arranged in the position shown in the figure when using
this manometer:
Valves must be arranged in the position shown in the figure when using
this manometer:
1. Fix the air and CO2 flow according to the method explained in the
operating mode section when both flow rates must be operated at the
same time and record the flow rates:
5% KOH solution
a. Check that the right hand branch of the U shaped tube (TU-U) is fully closed by its
top (no air can enter or leave through it during the practical exercise).
g. Repeat the steps 'c', 'd', 'e', 'f' till the KOH solution reaches a height between 70 and
100 mm in the scale located in the left hand branch of the U shaped tube (TU-U).
a. Connect the blower (AS-1) and let the air flow along the packed column (COL)
during a few minutes. Meanwhile:
b. Position the valve (VT-1) as shown in the figure and push the plunger of the syringe
(JE) to expel the air inside to the atmosphere.
c. Position the valves (VT-1, VT-2, VT-3 and VT-4) as shown in the figure:
Position of VT-5 to take samples from the UPPER part of the column:
f. Repeat the steps 'b', 'c', 'd', 'e' at least three times to obtain a representative sample
(please note that the first times only the air inside the tubes is taken, so the sample
will be representative after performing these steps several times).
g. Place the valve (VT-2) as shown in the figure:
i. Record the level of the solution in the left hand branch of the U shaped tube (TU-
U):
a. Push the plunger of the syringe (JE) slowly to introduce the gas sample in the KOH
solution vessel (it can be observed that the absorbing liquid is displaced to the
second vessel, and when stopping to push the plunger, the liquid goes back to the
left hand branch of the U shaped tube (TU-U)). Add the mixture slowly down to
the end of the syringe (JE). IMPORTANT: Do not introduce all the sample in
one go to prevent forcing the system and causing leaks.
b. When stopping to push the plunger of the syringe (JE) it can be observed that it
does not return to the initial position (100 ml if that was the sample taken for
), it remains above the initial value. It is due to the fact that part of the CO2 of
c. To see how much has been absorbed by the solution, pull the plunger VERY
SLOWLY until it indicates the initial level of the U shaped tube (TU-U), that is to
say, level recorded in the previous section (Taking a gaseous sample).
d. Keep the liquid from the left hand branch of the U shaped tube (TU-U) to that level
of and record the new volume indicated by the plunger of the syringe:
1. Once the reaction is produced the volume of CO2 from the sample that has been
absorbed by the KOH solution is calculated:
1. Arrange the valves (VT-2, VT-3, VT-4, V-10, V-11, VT-5) as shown in
the figure:
V-11
V-10
V-11 V-11
V-10 V-10
4. Wait till the measurement of the meter is stabilized (when it does not
change more than 1%).
a. Prepare a 0.02M NaOH solution. For that purpose dilute 0.32 g of NaOH in 400
ml of water.
b. Refill the burette with a certain amount of the previously prepared solution.
Record the initial volume of the burette:
Check that there are no leaks. Apply some grease to all the areas prone to
suffering leaks: o Plunger of the syringe o Valves o Connections of tubes with
hoses
Introduce the gas sample with the syringe (JE) in several strokes.
First, fix the water flow and let it run for one minute. Then, fix the air flow (for
the flooding practical exercise).
The software that corresponds to the CO2 meter must be installed in the CAGC
unit if the user wants to use that meter. The software is included in the CD of
the unit.
- Prevent the KOH solution from reaching a level in the U shaped tube (TU-U) very
close to the end of the scale, otherwise a certain amount of solution could pass
to the conduits of the gas samples taking lines and obstruct them.
- Use always the CO2 meter with the suitable safety measures,
that is to say, water trap, particles filter and humidity filter.
7.5.1 Practical exercises 1: Determination and plot of drag and flooding flows
7.5.1.1 Objective
To determine the conditions under which the column drag and flooding
process is generated and to plot the influence of the air and water flow rates variation on
the pressure inside the column.
2. Fix the water flow following the method described in the operating mode
section. It is recommended to start with low water flow rates, as for
example 30%.
5. Fix the air flow up to 10%, according to the method described in the
*In the CAGC unit the value of the circulating flow of air is given by
the sensor (SC-1).
6. Wait until the steady state is reached (pressure does not change with time).
7. Record the pressure drop suffered by the gas when crossing the column.
This value is obtained from the manometers of the panel (M-1 and/or M-2)
(see the operating method in the operating mode section):
*In the CAGC unit the pressure is indicated by the sensors: (SPD1)
for the entire column or (SPD-2) for the pressure of the lower half
of the column.
8. For every flow of liquid fixed, the pressure drop that correspond to
different air flow rates are measured (refer to the working sheet).
9. The natural logarithm for each flow rate and pressure drop recorded
before.
10.The logarithm of the pressure drop suffered by the gas when crossing
11.Repeat all the steps again when modifying the water flow rate.
IMPORTANT:
When the flooding starts, it is observed how the column (COL) is being filled
with water and the level rises gradually. Please, do not allow the water level
inside the column (COL) obstruct the orifices that communicate with the
manometers (M-1 and M-2) and sensors (SPD-1 and SPD-2), since they could
give wrong values. If they were eventually obstructed, stop the water pump (AB-
1) and open the regulation valve (VR-4) up to the maximum by turning it in
anticlockwise direction.
Please, take into account that high pressures will be reached for the flow rates
that generate the flooding. For that reason, use only the manometer (M-1 or M2)
with a liquid denser than water (the procedure to refill and discharge these
manometers is indicated in the annex).
10
20
30
40
50
60
70
10
20
30
40
50
60
70
10
20
30
40
50
60
70
Graph 1: Plot of the gas pressure drops through the packing: Drag and
flooding velocities.
Questions:
1. What occurs when the air flow rate is increased but the water flow rate is the
same?
3. Identify the different sections of each curve and explain what occurs in each
one.
PRACTICAL EXERCISES MANUAL
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7.5.2 Practical exercise 2: Analysis of gaseous currents using different methods
7.5.2.1 Objective
To analyze the amount of CO2 from a gaseous current using a solution of KOH.
- KOH solute
- Distilled water
- Stirrer
- Scale
2. Introduce the KOH solution in the U shaped tube (TU-U) (refer to the operating
mode section).
3. Fix the air and CO2 flow rate when both must be started at the same time according
to the method explained in the operating mode section and record the flow values:
4. Analyze the air current (there are three methods explained in the operating mode
section: theoretical method, analytical method and CO2 meter).
6. Analyze 3 or 4 gas samples as it was explained in the previous steps for fixed flow
rates of CO2 and air. Fill the working sheet attached below and answer the
questions.
Questions:
1. What does it happen when increasing the flow of CO2 for the same flow of air?
2. What does it happen when increasing the flow of air for the same flow of CO2?
3. For which flow rates is the lowest concentration of CO2 obtained? And the
highest concentration of CO2? Are the results logic? Explain your answer.
PRACTICAL EXERCISES MANUAL
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7.5.3 Practical exercise 3: Analysis of water samples
7.5.3.1 Objective
- Chemical elements:
o CO2
- Safety and prevention instrumentation: safety glasses, gloves, lab coat, etc.
1. Fix the flow of air and CO2 when both must be started at the same time according
to the method explained in the operating mode section and record the flow values:
4. Fix and regulate the water flow according to the operating mode and record the
flow value:
6. Put the hose that leaves from the valve (V-9) facing the water storage tank (TAA).
9. Watch and regulate the water level below the column (COL) with the valve (VR-4)
so that the level is between MAX. and MIN. IMPORTANT: this step must be
checked regularly when the valve (V-9) is opened or closed to take water
samples.
10. Put a beaker at the outlet of the hose that leaves through the valve (V-9) and fill it
with approximately 400 ml. At least three samples of 100 ml of water may be taken
and analyzed from this beaker for each fixed flow.
11. Prepare a solution of NaOH 0.02M. For that end dilute 0.32 g of NaOH in 400 ml
of distilled water.
12. Refill the graduated burette with a certain amount of the previously prepared
solution. Record the initial volume of the burette:
13. Pour the water sample to be analyzed in an Erlenmeyer flask of 100 ml.
14. Add 10 drops of phenolphthalein indicator. If the sample turns pink, there is no
CO2. If the sample remains colorless, add drop by drop the NaOH solution
17. Note down and adjust the reaction that takes place:
21. Then, record the volume of NaOH solution employed for the titration of each
water sample and calculate the average volume used:
26. Repeat all the steps for different flows of water, air and CO2, as the ones
shown in the table below, and answer the questions.
50 30
30 30 1,3
30 50
50 30 2
30 30 2,6
30 50
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7.5.3.1 Working sheet
Questions:
1. What happens when increasing the flow of CO2 for the same flow of air and
water?
2. What happens when the air flow is increased for the same flow of CO2 and
water?
3. What happens when the water flow is increased for the same flows of air and
CO2?
4. For which flows is the lowest concentration of CO2 obtained? And the highest
concentration? Are the results logical? Explain the answer.
PRACTICAL EXERCISES MANUAL
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7.5.4 Practical exercise 4: Determination of the mass transfer coefficient for a
packed column
7.5.4.1 Objective
Determination of the mass transfer overall mean volumetric coefficients through the
liquid phase and the influence of the flow of liquid on that coefficient.
In our case, as the control is exerted by the liquid phase (water in this case)
it will only be necessary to determine the mass transfer coefficient through the liquid
phase ( ).
- Safety and prevention instrumentation: safety glasses, gloves, lab coat, etc.
1. Fix the flow of air and CO2 when both must be started at the same time according
to the method explained in the operating mode section
4. Determine the total flow of gas G (air and CO2) at the inlet of the column (COL)
in the lower part:
5. Analyze the air current according to the method explained in the operating mode
section (theoretical method, analytical method and/or meter) and record the mole
concentration of CO2 of the sample before starting the water circuit:
8. Fix and regulate the water flow according to the operating mode section.
9. Wait 5 minutes until reaching the stationary state and control the water level
below the tank. At that moment the absorption of CO2 in the water will start.
Put the hose that leaves from the valve (V-9) directed towards the water storage tank
(TAA).
Open the valve (V-9) and allow the flow of water through the hose towards the tank
(TAA).
Watch and regulate the water level below the column (COL) with the valve (VR-4)
so that the level is between MAX. and MIN.
Put a beaker at the outlet of the hose that leaves from the valve (V-9) and fill it with
a little bit more than 300 ml.
Three samples of 100 ml of water can be taken from the beaker for each
established flow and analyze them (refer to acid-base titration in the operating mode
section). Then record the volume of NaOH solution employed for titrating each
water sample and calculate the average volume employed:
Obtain the flow of CO2 transferred to the water (coefficient N that will allow the
student to calculate the transfer coefficient (KL)):
1. Calculate the partial pressures before and after water flows through the column:
specific area of packing per unit of volume of packing (m2/m3). For the
size of Raschig rings employed: a = 440 m2/m3.
Table 6: Calculation of the total flow of liquid (water) that crosses the column
(COL) and determination of the mole fractions at the outlet (x2 and y2) of the column
(COL).
N=flow of
Molarity moles CO2
Nº Water L ml of NaOH used CO2 in (x2)
Average of the in 100ml
Exp. (l/min) (kg/min) in the titration water measured
sample sample
(mol/s)
2 1,3
5 2,6
6
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109
7.5.4.4 Working sheet
6
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109
7.5.4.4 Working sheet
Questions:
1. What happens when increasing the flow of CO2 for the same flow of air and water?
2. What happens when increasing the flow of air for the same flow of CO2 and water?
3. What happens when increasing the flow of water for the same flows of air and CO2?
4. In which case is the mass transfer coefficient higher? And lower? Explain the
answer.
5. In your opinion, how should an industrial packed column be to obtain a greater mass
transfer?
6. Which type of gases could be employed to detect absorption? High solubility or low
solubility gases?
PRACTICAL EXERCISES MANUAL
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7.5.5 Practical exercise 5: Mass balance verification
7.5.5.1 Objective
Check that the mass balance is verified for the packed column (COL).
Mass balance:
Where,
(nondimensional)
Mole fraction of CO2 in the mixture (air + CO2) at the inlet
of the column (COL) (lower part)
(nondimensional)
Mole fraction of CO2 in the water at the inlet of the column
(COL) (upper part). It is practically non-existent, water does
not have CO2.
(nondimensional)
Mole fraction of CO2 in the water at the outlet of the column
(COL) (lower part)
1. Calculate the mole fraction at the outlet of the column (COL) (upper
part) y2 from the mass balance with the results obtained in the practical
exercise 4 (Calculation of the mass transfer coefficient) and compare
them with the y2 of the meter:
Questions:
Nº G L (y2)
EXP (g/min) (g/min) (x1) (x2) measured
1
2
3
4
5
6
3. If there is any difference, what might it be due to? Explain the answer.
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7.6 ANNEXES
7.6.1 Assembly
- Analysis panel.
- Packed column.
The packed column and part of the liquid circuit of the bottom of the
column are disassembled for the delivery of the unit. The procedure to mount the column
and the water circuit is described below:
1 2
3 4
COLUMN
NARROWING
3. Introduce the packing in the column. The packing is Raschig rings of 10x10mm
that must be supported by the PVC plate placed in the previous step. The
packing level must not be higher than the black gasket at the top nor be in
contact with the glass diffusion shower. The ideal height is 5 cm below the
black gasket.
Packing
5. Locate the column in its place taking into account that the white gasket made
of Teflon must be correctly located so that there are no leaks. Put the black
flange at the bottom with the black float inside.
White Teflon
gasket
2. Locate it at the bottom of the valve (V-7) and introduce the silicon tube in the vessel
that contains the liquid.
3. Place the valve (VT-1) as shown below and push the plunger of the syringe (JE) to
expel the air inside to the atmosphere.
7. Close the valve (V-7) and rotate the valve (VT-1) in such a way that the manoneter
(M-1) connect with the atmosphere, thus, the liquid inside will be evenly
distributed between both branches:
2. Locate it at the bottom of the valve (V-8) and introduce the silicon tube in the
vessel that contains the liquid.
3. Place the valve (VT-1) as shown below and push the plunger of the syringe (JE)
to expel the air inside to the atmosphere.
7. Close the valve (V-8) and rotate the valve (VT-1) in such a way that the
manometer (M-1) connect with the atmosphere, thus, the liquid inside will be
evenly distributed between both branches:
Reason: The full stroke of the syringe is not enough to make all the required
amount of solution rise in one time.
Solution: Read how to introduce the solution in the U tube (TU-u) in the
operating mode section.
Pushing the plunger of the syringe requires much effort (JE).
Reason: The gas sample and the liquid are in a closed circuit, there must be no
leaks.
Solution: Seal all connections with grease, specially the area surrounding the
plunger of the syringe (JE) and the tubes and hoses connections.
The column is not flooded.
Solution: First, fix the water flow rate, leave it run for at least one minute and,
then, fix the air flow rate.