In The Name of Allah

Petroleum University of Technology

Dept. of Chemical Engineering

Prepared by:
Dr. R. M. Behbahani
M. Nazari
Sep. 2011
A Introduction

Liquid Phase
Chemical
Reactor

Warnings

 Before the equipment is used for experiments, flush the system with distilled water to
remove all traces of possible chemical contamination.
 To use the mixer: turn the speed controller fully clockwise to start the stirrer, then
reset to the desired speed setting.
 At the end of four experiments, please:
A) Switch off all electrical items on the equipment.
B) Remove all water from the feed tank, reactor vessel and sump tray using the
appropriate drain cocks.

Petroleum University of Technology / Unit Operation Laboratory A-1

A Experiment No.1

Liquid Phase
Chemical
Reactor

Aim: the analysis of reactants and products for a saponification reaction by titration.

Procedure:

1. Mix 250 ml of standardized 0.1 M, NAOH with 250 ml of standardized o.1 M, EtoAC
in a 1 liter flask and secure stopper, after about one hour take a 10 ml sample and
place in titration flask.
2. Neutralize this sample with 10.0 ml of 0.1 M HCl.
3. Titrate this mixture with 0.1 M, NaOH until the end point is reached. Note volume
used.
4. Repeat the above procedure for two other samples.

Calculations:

1. Find the concentration of unreacted NaOH in samples.

2. Comment upon the results obtained.

Petroleum University of Technology / Unit Operation Laboratory A-2

A Experiment No.2

Liquid Phase
Chemical
Reactor

Aim: To find the order of the reaction and a value of the reaction rate constants in a
stirred batch reactor for the saponification of ethyl acetate with dilute sodium
hydroxide.

Procedure:

1. One liter of each of the made up solutions of 0.1 M sodium hydroxide and 0.1M
Eto AC should be mixed at room temperature at an arbitrary time (t = 0) in the
stirred reactor.
2. At various subsequent times, a sample of the mixture of 25 ml. should be
withdrawn and the unreacted NaOH neutralized with 25 ml. (or less) 0.1M
hydrochloric acid.
3. Back-titrate the above solutions with 0.1 M sodium hydroxide to determine the
conversion of ETo AC in the reactor. This must be carried out as rapidly as possible
to avoid acid hydrolysis of the acetate. The temperature of the vessel contents should
be noted.
4. Repeat the above procedure at four other temperatures.

Calculations:

From the data obtained:

a) Plot the volume of unused NaOH V.S. time (min.)

b) Find the order of the reaction and the value of the reaction rate constant in a stirred
batch reactor (k).
c) Investigate the relationship between the specific rate constant (k) and the temperature
of reaction. Comment upon the results obtained.

Petroleum University of Technology / Unit Operation Laboratory A-3

A Experiment No.3

Liquid Phase
Chemical
Reactor

Aim: To find the reaction rate constant in a continuous stirred tank reactor for
saponification of ethyl acetate with dilute NaOH.

Procedure:

1. Fill each of the feed tanks A and B with 15 liters of 0.1 M, ETo AC and 0.1M, NaOH
solutions, respectively.

2. Adjust both flow control valves to deliver about 40 ml. /min. of each of the reactants
to the stirred reactor. Continue until S.S. flow is reached.

3. At various times collect 25 ml. samples of the reactor overflow and neutralize the
residual NaOh with a known amount of excess 0.1 M, HC1.

4. Back-titrate the above solutions with 0.1 M, NaOH, to determine the conversion of
Eto AC in the reactor. This must be carried out as rapidly as possible to avoid acid
hydrolysis of the acetate. The temperature of the reactor vessel should be noted.

Calculations:

1. Write a mass balance around the stirred reactor vessel and find the equation for the
rate constant in a continuous stirred reactor.

2. From the data obtained:

a) Plot the concentration of NaOH in the reactor V.S. time.

b) Find the specific rate constant in a continuous stirred reactor.

Comment upon the results obtained.

Petroleum University of Technology / Unit Operation Laboratory A-4

A Experiment No.4

Liquid Phase
Chemical
Reactor

Aim: To investigate the effect of inadequate mixing on the reaction rate of EtoAC with dilute
NaOH in a batch reactor.

Procedure:

1. Mix one liter of each of the made up solutions of 0.1 M sodium hydroxide and 0.1 M
ethyl acetate, at room temperature in the stirred reactor fitted with baffles.

2. At various times, take a 25 ml. sample of the mixture, and neutralize its residual
NaOH with a known volume of excess 0.1 M, HC1.

3. Back-titrate the above samples with 0.1 M, NaOH solution to determine the
conversion of ethyl acetate in the reactor. This must be carried out as rapidly as possible to
avoid hydrolysis of the acetate.

4. Repeat the experiment, while removing the baffle but using the same stirrer speed as above.

5. Repeat the experiment again without the baffle and with no stirring of the mixture.

NOTE:

It is essential to maintain the temperature, constant throughout all these tests.

Calculations:

1. From the data obtained:

Plot the conversion of ETo AC V.S. time for each speed of stirring, (including with & without
baffles and stirring)

Petroleum University of Technology / Unit Operation Laboratory A-5

A Experiment No.4

Liquid Phase
Chemical
Reactor

2. Comment on the results obtained.

Questions:

1. How did removal of the baffle affect the reaction rate?

2. What effect does stirring have on the reaction rate?

Petroleum University of Technology / Unit Operation Laboratory A-6

B Experiment No.1

Diffusion
Coefficient
Determination

Aim: To determine the diffusivity of acetone vapour in the air, and to investigate the effect of
temperature on the diffusivity coefficient.

Theory:

Consider a fluid (either liquid or gas) which is a mixture of two components A and B. The resistance to
diffusion of the component A through the solution will be proportional to:

a) The relative velocities of A & B i.e. to (UA-UB).

b) The distance through which diffusion occurs, dz.

c) The number of molecules of A & B in the path of diffusion. This in turn, is proportional to the
concentrations of the species, i.e. to CA, CB.

d) The driving force or potential which overcomes this resistance, namely the
concentration gradient of species A over the distance dZ, i.e. dCA.

Combining all the above terms, gives:

dcA = -bCACB (UA - UB) dZ (1)
where b is the proportionality constant.

This is the fundamental diffusion equation for the rate of diffusion of a single component
through a fluid mixture. It is known as the "Stefan-Maxwell Equation".

Equations for steady-state diffusion of only one of the two species in binary mixtures of ideal
solutions are readily obtained from Eq. (1), which reduces to:

(2)

Petroleum University of Technology / Unit Operation Laboratory B-1

B Experiment No.1

Diffusion
Coefficient
Determination

The above steady-state equations for molecular diffusion may be used with little error in
many situations where conditions are changing with time. Unfortunately, it is often quite
difficult to determine the error involved in doing this; the exact solution is needed to estimate
the error and would be used if obtainable and simple.

Procedure:

One experimental method of measuring DAB in binary gas systems is to place a liquid A at
the bottom of a tube of small diameter containing a gas B. Pure B is passed slowly over the
top end of the tube, thus maintaining the partial pressure PA2 Zero at that point. The partial
pressure PA1 in the gas adjacent to the liquid surface is assumed equal to the vapor pressure of
A at the temperature of the experiment. Diffusion of A through B occurs in the gas filled
tube of the varying length Z. The rate of diffusion is determined is determined by the rate of
fall of the level of the liquid, which has a known molal density M.

Though this is clearly a case of transient diffusion, the data obtained are usually interpreted
by equating the steady-state flux, as given by Eq. (2), to the rate of vaporization:

 (3)


(4)

where ZQ and Zt are the heights of the gas space at t=0 and t=t respectively.

Petroleum University of Technology / Unit Operation Laboratory B-2

B Experiment No.1

Diffusion
Coefficient
Determination

NOTE:

The use of the steady-state expression introduces two errors: (1) the distribution of A through
the gas space at the beginning of the test may be quite different from that prevailing under
steady-state conditions, and (2) some of the observed drop in liquid level Produces vapor
which occupies the space originally filled with liquid and does not diffuse out of the tube.

These errors are very small. Lee and Wilke [4] have shown the first to be small by an
analysis of the transient approach to the steady-state flux. The second is evidently small
because the partial density of A in the space is so small compared with that of the liquid. A third
minor error due to the radial velocity gradients in the vapor moving upward in the tube is discussed by
Rao and Bennett [5].

Calculations:

1. Determine the diffusivity of acetone vapour in the air.

Questions:

1. Develop Eq. (4) from "Stefan- Maxwell equation".

References:
1) Perry, J.H.: Chemical Engineering Handbook, 5th ed., Mc Graw Hill, New York, 1980.
2) Sherwood, T.K., Pigford R.L. and Wike C.R.: Mass Transfer, Mc Graw Hill, New York,
1975.
3) Wilke, C.R. and Chang P.: AICHE J., 1: 264 (1955).
4) Lee, C.Y. and Wilke C.R.: Ind. Engineering Chemical, 46: 2381 (1954).
5) Rao, S.S., and Bennett C.O.: Ind. Engineering Chemical, 5: 573 (1966).

Petroleum University of Technology / Unit Operation Laboratory B-3

C Introduction

Liquid-Liquid
Extraction

Many processes in chemical engineering require the separation of one or more of the
components of a liquid mixture by treating the mixture with an immiscible solvent in which
these components are preferentially soluble. In some cases purification of a liquid may be the
function of the process, in others the extraction of a dissolved component for subsequent
processing may be the important aspect. An example of the former is the preparation of pure
organic liquids from products of the oil industry. Liquid/liquid extractions may also be used
as energy-saving processes by, for example, eliminating distillation stages. It is possible, of
course that the substance of interest may be heat-sensitive anyway and that distillation is
accordingly an unacceptable process.

The rate at which a soluble component is transferred from one solvent to another will be
dependent, amongst other things on the area of the interface between the two immiscible
liquids. Therefore it is very advantageous for this interface to be formed by droplets and
films, the situation being analogous to that existing in packed distillation columns.

Fig C.1. Liquid-liquid Extraction unit Fig C.2. Control and instrumentation

Petroleum University of Technology / Unit Operation Laboratory C-1

C Experiment No.1

Liquid-Liquid
Extraction

Aim: To determine the distribution coefficient for the system organic solvent-Propionic Acid-
Water and to show its dependence on concentration.

Theory:
The solvent (water) and solution (organic solvent/propionic acid) are mixed together and then
allowed to separate into the extract phase and the raffinate phase. The extract phase will be
water and propionic acid and the raffinate, organic solvent with a trace of propionic acid.
The distribution coefficient, K, is defined as the ratio:

It is assumed that equilibrium exists between the two phases. At low concentrations, the
distribution coefficient is dependent on the concentration and thus Y = KX.

Procedure:

Equipment Set-Up:

The following apparatus is required:

 250ml Conical stoppered flask
 250ml Measuring cylinder
 250ml Separating funnel
 Pipette with rubber bulb
 Sodium Hydroxide Solution (0.1 M)
 Phenolphthalein
 Propionic acid

Petroleum University of Technology / Unit Operation Laboratory C-2

C Experiment No.1

Liquid-Liquid
Extraction

Reading to be taken:
1. Make up in a conical flask a mixture of 50ml organic solvent and 50ml of de-
mineralized water.
2. Add 5ml of propionic acid. 5ml can be pipetted into the flask using a pipette with a
rubber bulb.
3. Place a stopper into the flask and shake for a minimum of 5 minutes.
4. Pour into a separating funnel, leave for 5 minutes and remove the lower aqueous
layer.
5. Take a 10ml sample of this layer and titrate against 0.1 M sodium hydroxide solution
using phenolphthalein as indicator.
6. Repeat the experiment for two further concentrations of propionic acid i.e. for initial
additions of 3ml and 1ml of propionic acid.

RESULTS:

Calculations:

1. Fill out the calculated data in the table.

2. Plot the results as Y versus X producing an equilibrium curve.
3. Plot the results in triangle diagram to prepare an equilibrium curve.

Petroleum University of Technology / Unit Operation Laboratory C-3

C Experiment No.2

Liquid-Liquid
Extraction

Aim: To observe the hydraulics of counter current flow in a packed column.

Theory:
It is normal to operate a column so that the continuous phase 'wets' the packing. If the
packing is 'wetted' by the dispersed phase then coalescence will be increased and the mass
transfer/unit volume will be reduced. The rate of mass transfer of a solute from one phase to
another is normally increased with greater throughput of material, because of increased
turbulence giving better mixing. There is however, a limit to the maximum amount of
material that can be fed through the column. The limit is called the 'Flooding Point' and
occurs at specific flow rates of constituents resulting in one of the phases being rejected from
the column.

Procedure:

Equipment Set-Up:

The experiment will be carried out using the two immiscible liquids organic solvent and
water and the column will be operated in the following two modes:
(a) The aqueous phase as the continuous medium.

(b) The organic phase as the continuous medium.

The solvent metering pump is calibrated in percentage of maximum flow which varies
slightly from pump to pump. The pump should be calibrated initially by setting F2 to 100%,
setting valve V8 to the calibrate position and measuring the flow from the pump, using a
measuring cylinder and stopwatch. Calculate the flow rate produced settings of 5% intervals
(ml per minute), then plot a graph of ml per minute against percentage of metering pump
stroke. Thereafter any selected flow may be obtained by using the graph.

NOTE:

To prevent damage to the solvent pump, always make sure that the pump is switched off
before changing the position of the calibration.

Petroleum University of Technology / Unit Operation Laboratory C-4

C Experiment No.2

Liquid-Liquid
Extraction

Fig C.3. Aqueous phase as continues medium (a)

Fig C.4. Organic phase as continues medium (b)

Petroleum University of Technology / Unit Operation Laboratory C-5

C Experiment No.2

Liquid-Liquid
Extraction

1. The Aqueous Phase as the Continuous Phase

1. Fill the organic phase feed tank (bottom tank) with 10 liters of trichloroethylene.
2. Fill the water feed tank with 15 liters of clean de-mineralized water, start the
water feed pump (switch S3) and fill the column with water at a high flow rate.
3. As soon as the water is above the top of the packing, reduce the flow rate to 0.2
l/min (using the calibration graph obtained as described above) and switch on the
conductivity probe at the bottom of the column (selector switch to 'down'
position).
4. Start the organic phase metering pump and set at a flow rate of 0.2 l/min (switch
S4). Wait until column overflows.
5. Slowly increase both water and organic solvent flow rates and note where
flooding occurs.

(b) The Organic Phase as the Continuous Phase

6. Empty the column and return the organic solvent and water into their respective
feed tanks. This is achieved by allowing the weight of the water to push the
organic solvent to the solvent collection tank (top tank), (this may mean adding
more water). Then draining column and L1, L2 - refilling L2. Switch off the top
conductivity probe (switch S2 in the centre position).
7. Start the metering pump (switch 4) and fill the column quickly, regulate to a flow
of 0.2 L/min when organic solvent reaches the top of the packing. Switch S2 to
the up position.
8. Switch on the water pump (switch S3) and regulate the flow 0.2 L/min
9. Slowly increase the flow rates until flooding occurs.

Questions:

Observe if there is any difference between operating with the aqueous phase as the
continuous medium compared with the organic phase as the continuous medium.

Petroleum University of Technology / Unit Operation Laboratory C-6

C Experiment No.2

Liquid-Liquid
Extraction

Is there any difference in droplet size? Also observe what happens as the flow rates are
increased. Does flooding occur, if so at what flow rates?

Petroleum University of Technology / Unit Operation Laboratory C-7

C Experiment No.3

Liquid-Liquid
Extraction
Aim: To demonstrate how a mass balance is performed on the extraction column, and to
measure the mass transfer coefficient with the aqueous phase as the continuous medium.

Theory:

The theory is given for the system Kerosene-propionic acid-water.

Let Vw: Water flow rate (l/s)

Vo: Organic solvent flow rate (l/s)

X: Propionic Acid concentration in the organic phase (kg/l)

Y: Propionic Acid concentration in the aqueous phase (kg/l)

Subscripts:

1: Top of column
2: Bottom of column

1. MASS BALANCE
Propionic Acid extracted from the organic phase (raffinate) = Vo (X2-X1)

Propionic Acid extracted by the aqueous phase (extract) = Vw(Y1-0)

Now Vo(X2-X1) = Vw(Y2-0)

2. EXTRACTION EFFICIENCY

Mass transfer coefficient (based on the raffinate phase)

Petroleum University of Technology / Unit Operation Laboratory C-8

C Experiment No.3

Liquid-Liquid
Extraction

where ΔX1 = Driving force at the top of the column = (X1- 0)

ΔX2 = Driving force at the bottom of the column = (X2-X2*)

where X2* is the concentration in the organic phase which would be in equilibrium with

concentration Y2 in the aqueous phase. The equilibrium values can be found using the

distribution coefficient found in the first experiment.

Procedure:

Equipment set-up:

The solvent metering pump is calibrated in percentage of maximum flow which varies
slightly from pump to pump. The pump should be calibrated initially by setting F2 to 100%,
setting valve V8 to the calibrate position and measuring the flow from the pump, using a
measuring cylinder and stopwatch. Calculate the flow rate produced settings of 5% intervals
(ml per minute), then plot a graph of ml per minute against percentage of metering pump
stroke. Thereafter any selected flow may be obtained by using the graph.

Fig C.5. Aqueous phase as continues medium

Petroleum University of Technology / Unit Operation Laboratory C-9

C Experiment No.3

Liquid-Liquid
Extraction

1. Add 100ml of propionic acid to 10 liters of the organic phase. Mix well to ensure an even
concentration then fill the organic phase feed tank (bottom tank) with the mixture.
2. Switch the level control (electrode switch S2) to the OFF (central) position.
3. Fill the water feed tank with 15 liters of clean de-mineralized water, start the water feed
pump and fill the column with water at a high flow rate.
4. As soon as the water is above the top of the packing, reduce the flow rate to 0.2 l/min
(using the calibration graph obtained as described above).
5. Set electrode switch S2 to the bottom position. Start the metering pump and set at a flow
rate of 0.2 l/min.
6. Run for 15-20 minutes until steady conditions are achieved, monitor flow rates during this
period to ensure that they remain constant.
7. Take 15ml samples from the feed, raffinate and extract streams. DO NOT use the
calibration valve V8 for taking feed samples.
8. Titrate 10ml of each sample against 0.1 M NaOH using phenolphthalein as the indicator.

RESULTS:

Petroleum University of Technology / Unit Operation Laboratory C-10

C Experiment No.3

Liquid-Liquid
Extraction

Calculations:

Fill out the calculated data in the table.

Petroleum University of Technology / Unit Operation Laboratory C-11

C Experiment No.4

Liquid-Liquid
Extraction

Aim: To demonstrate how a mass balance is performed on the extraction column, and to
measure the mass transfer coefficient with the organic phase as the continuous medium.

Theory:

The theory is given for the system Kerosene-propionic acid-water.

Let Vw: Water flow rate (l/s)

Vo: Organic solvent flow rate (l/s)

X: Propionic Acid concentration in the organic phase (kg/l)

Y: Propionic Acid concentration in the aqueous phase (kg/l)

Subscripts:

1: Top of column
2: Bottom of column

1. MASS BALANCE
Propionic Acid extracted from the organic phase (raffinate) = Vo (X2-X1)

Propionic Acid extracted by the aqueous phase (extract) = Vw(Y2-0)

Therefore Vo(X2-X1) = Vw(Y2-0)

2. EXTRACTION EFFICIENCY

Mass transfer coefficient (based on the raffinate phase)

Petroleum University of Technology / Unit Operation Laboratory C-12

C Experiment No.4

Liquid-Liquid
Extraction
where ΔX1 = Driving force at the top of the column = (X1- 0)

ΔX2 = Driving force at the bottom of the column = (X2-X2*)

where X2* is the concentration in the organic phase which would be in equilibrium with

concentration Y2 in the aqueous phase. The equilibrium values can be found using the

distribution coefficient found in the first experiment.

Procedure:

Equipment set-up:

The solvent metering pump is calibrated in percentage of maximum flow which varies
slightly from pump to pump. The pump should be calibrated initially by setting F2 to 100%,
setting valve V8 to the calibrate position and measuring the flow from the pump, using a
measuring cylinder and stopwatch. Calculate the flow rate produced settings of 5% intervals
(ml per minute), then plot a graph of ml per minute against percentage of metering pump
stroke. Thereafter any selected flow may be obtained by using the graph.

Fig C.6. Organic phase as continues medium

Petroleum University of Technology / Unit Operation Laboratory C-13

C Experiment No.4

Liquid-Liquid
Extraction
1. Fill the organic phase feed tank with 10 liters organic phase and 10 ml of propionic
acid.
2. Switch the level control (electrode switch S2) to the OFF (central) position.
3. Fill the water feed tank with 10 liters of clean de-mineralized water, start the water
feed pump and fill the column with water at a high flow rate.
4. As soon as the water is above the top of the packing, reduce the flow rate to 0.2 l/min
(using the calibration graph obtained as described above).
5. Set electrode switch S2 to the bottom position. Start the metering pump and set at a
flow rate of 0.2 l/min.
6. Run for 15-20 minutes until steady conditions are achieved, monitor flow rates during
this period to ensure that they remain constant.
7. Take 15ml samples from the feed, raffinate and extract streams. DO NOT use the
calibration valve V8 for taking feed samples.
8. Titrate 10ml of each sample against 0.1 M NaOH using phenolphthalein as the
indicator.

RESULTS:

Petroleum University of Technology / Unit Operation Laboratory C-14

C Experiment No.4

Liquid-Liquid
Extraction

Calculations:

Fill out the calculated data in the table.

Petroleum University of Technology / Unit Operation Laboratory C-15

D Introduction

Gas
Absorption
Column

The packed tower, in which two fluids flowing in opposite directions enable a chemical
component to be transferred from one fluid phase to the other, occurs in almost all chemical
plants. The process may be gas absorption, distillation, solvent extraction or chemical
reaction. Knowledge of the characteristics of both fluid flow and of mass transfer in such
towers is necessary for both plant operators and designers.

The Armfield Gas Absorption Apparatus has

been designed to allow these studies to be
made and the instrumentation and layout
enables students to follow both the
hydrodynamic characteristics in the absence of
mass transfer, and also, separately, to advise
the performance of the mass transfer process
involved in gas absorption. The size of the
equipment has been chosen so that
experiments may be completed in a typical
laboratory class period, while at the same time
being capable of demonstrating full-scale
plant behavior. Considerable attention is
directed towards matters of safety which is of
crucial importance in the process industries.

Fig D.1. Gas Absorption column

Petroleum University of Technology / Unit Operation Laboratory D-1

D Experiment No.1

Gas
Absorption
Column

Aim: To determine the air pressure differential across the dry column as a function of the air
flow rate.

Procedure:

Equipment Set-Up:

Absorption column

1. The column must be dried by passing the maximum air flow until evidence of
moisture in the packing has disappeared.
2. Connect the column top and bottom of the water manometer with the stopcocks S1
and S3.
3. Take monometer reading of pressure differential across the column for a range of air
flow rates.

Petroleum University of Technology / Unit Operation Laboratory D-2

D Experiment No.1

Gas
Absorption
Column

Reading to be taken:

Air flow rate (l/m) 50 80 100 120 140 160 180 200

Pressure Differential (mm H2O)

Calculations:

Plot the pressure differential as a function of air flow rate on log-log graph paper and
establish the relationship between these variables.

Petroleum University of Technology / Unit Operation Laboratory D-3

D Experiment No.2

Gas
Absorption
Column

Aim: To examine the air pressure differential across the column as a function of air Flow
rate for different water flow rates on the column.

Procedure:

Equipment Set-Up:

Absorption column

1. Fill the water reservoir tank to three-quarters full with tap water.

2. Switch on the water pump and set C1 to give a flow rate of say 3 liters/minute down
the column.

3. After about 30 seconds close C1 switch off the pump and allow the column to drain
for 5 minutes.

Petroleum University of Technology / Unit Operation Laboratory D-4

D Experiment No.2

Gas
Absorption
Column

4. Measure the air pressure differential across the wet column as a function of the air
flow rate.

5. Measure the air pressure differential across the column as a function of the air flow rate for
different water flow rates up to say 5 liters/minute, noting the appearance of the column at
each setting.

Reading to be taken:

Air flow
l/m 20 40 60 80 100 120 140 160 180 190 200
Water flow
l/m

2.5

3.0

3.5

NOTE:

The range of possible air flow rates will decrease with increasing water flow rate due to onset
of "flooding" of the column, which should be noted.

Petroleum University of Technology / Unit Operation Laboratory D-5

D Experiment No.2

Gas
Absorption
Column

Calculations:

Pressure differential should be plotted as a function of air flow rate on log-log graph paper for
each water flow rate. It may be necessary then, to take more readings in order to define
precisely the transition points on the resulting graphs.

Petroleum University of Technology / Unit Operation Laboratory D-6

D Experiment No.3

Gas
Absorption
Column
Aim: To calculate rate of absorption of carbon dioxide into water from analysis of liquid
solution flowing down absorption column.

Procedure:

Equipment Set-Up:

1. Fill the liquid reservoir tank at the base of the column to approximately three-quarters
full with (preferably) deionised water. Note the volume added [VT liters] .

2. With gas flow control valves C: and C3 closed, start the liquid pump and adjust the
water flow through the column to approximately 6 liters/minute on flow meter F t by
adjusting flow control valve C1.

3. Start the compressor and adjust control valve C2 to give an air flow of approximately
10% of full scale on flow meter F2.

Petroleum University of Technology / Unit Operation Laboratory D-7

D Experiment No.3

Gas
Absorption
Column
4. Carefully open the pressure regulating valve on the carbon dioxide cylinder, and
adjust valve C3 to give a value on the flow meter F3 approximately one half of the air
Flow F2. Ensure the liquid seal at the base of the absorption column is maintained by,
if necessary, adjustment of control valve C4.

5. After 15 minutes of steady operation, take samples at 10 minute intervals from S4 and
Ss. Take 150ml samples at known times in each case. Analyze the samples according
to the procedure detailed below.
Analysis of Carbon Dioxide Dissolved in Water

NOTE:

Water used for absorption should be deionised as presence of dissolved salts affect the
analysis described below. If tap water is used, no metal ions should be present in greater
quantities than 1.5 mg/liter and pH should be just alkaline: 7.1 to 7.8.

1. Chemical Solutions Needed:

a. Phenolphthalein indicator prepared from carbon dioxide free distilled water i.e. A. R.
grade.
b. Standard 0.0277M sodium hydroxide solution prepared by diluting 27.70ml 1M
caustic soda standard solution to 1 liter with carbon dioxide free distilled water.
Prepare daily and protect from carbon dioxide in the atmosphere by keeping in a
stoppered Pyrex bottle.
c. Standard 0.01M sodium bicarbonate solution, prepared by dissolving approximately
0.1 gram of anhydrous sodium bicarbonate in carbon dioxide free distilled water to
100ml.
2. Procedure:
1. Withdraw a sample of liquid Ss from the sump tank with the sampler provided,
approximately volume of 150ml, or from liquid outflow point S4.
2. Discharge the sample at the base of a 100ml graduated cylinder, flicking the
cylinder to throw off excess liquid above the 100ml mark.

Petroleum University of Technology / Unit Operation Laboratory D-8

D Experiment No.3

Gas
Absorption
Column

3. Added 5-10 drops of phenolphthalein indicator solution A. above; if the sample

turns red immediately, no free CO2 is present. If the sample remains colorless,
titrate with standard alkali solution B. above; Stir gently with a glass rod until a
definite pink color persists for about 30 second. This color changed is the end
point - note volume VB of alkali solution added.

For best results, use a color comparison standard, prepared by adding the identical
volume of phenolphthalein solution a) to 100ml of sodium bicarbonate solution C. in
a similar graduated cylinder.

3. Calculation:

The amount of free CO2 dissolved in the water sample is calculated from:

NOTE:

Solubility of C02 in water is a strong function of temperature.

The accuracy of this titrimetric method is approximately 10%.

Reading to be taken:

F1: …………….. Liters/second

VT: …………… volume of water in system (liters)

Petroleum University of Technology / Unit Operation Laboratory D-9

D Experiment No.3

Gas
Absorption
Column

From sump tank S5

From liquid outlet sample point S4
Time from (correspond to conditions at top of tower)
start VB ml. Cd in tank VB ml. Cd at outlet
(minutes) [Cdi] g. mole / liter [Cd0] g. mole / liter
10
20
30
40
50
60

Calculations:

1. CO2 absorbed over a time period (e.g. 30 minutes):

2. CO2 absorbed across the column at any particular time:

Inlet flow of dissolved CO2 = F1.Cdi g.mole/second
Outlet flow of dissolved CO2 = F1.Cd0 g.mole/second
i.e. Absorption rate = Fi.[Cdi-Cdo] g.mole/second

Petroleum University of Technology / Unit Operation Laboratory D-10

D Experiment No.4

Gas
Absorption
Column

Aim: To measure the absorption of carbon dioxide into water flowing down the tower, using
the gas analysis equipment provided /Hemple apparatus/.

Procedure:

Equipment Required:

a. Carbon dioxide cylinder with integral pressure regulator, connected to regulator R on

gas inlet on the apparatus.
b. Approximately 300ml of 1.0 molar caustic soda solution with safety gloves and
goggles, small funnel and tubing for tilling analysis equipment.

Equipment Set-up:

1. First fill the two globes of the absorption analysis equipment on the left of the panel
with 1.0 Molar caustic soda. Wear gloves and goggles while doing this. Adjust the
level in the globes to the '0' mark on the sight tube, using drain valve Cv into a flask to
do this.
2. Fill the liquid reservoir tank to three quarters full with fresh tap water.

Petroleum University of Technology / Unit Operation Laboratory D-11

D Experiment No.4

Gas
Absorption
Column

3. With gas flow control valve C2 and C3 closed, start the liquid pump and adjust the
water flow through the column to approximately 6 liters / minute on flow meter F1 by
adjusting control valve C1.
4. Start the compressor and adjust control valve C2 to give airflow of approximately 30
liters /minute in flow meter F2.
5. Carefully open the pressure regulating valve on the carbon dioxide cylinder, and adjust
valve C3 to give a value on the flow meter F3 approximately one half of the air flow F2
Ensure the liquid seal at the base of the absorption column is maintained by, if
necessary, adjustment of control valve C4.
6. After 15 minutes or so of steady operation, take samples of gas from the top and
middle sample points. (Refer to the appropriate diagram for details of the valve
positions) Analyze these consecutively for carbon dioxide content in these gas samples
as shown in the accompanying sketch and following notes.
7. Flush the sample lines by repeated sucking from the line, using the gas piston and
expelling
the contents of the cylinder to atmosphere. Note that the volume of the cylinder is
about 100cc. Estimate the volume of the tube leading to the device. Then decide how
many times you need to suck and expel.
8. With the absorption globe isolated and the vent to atmosphere closed, fill the cylinder
form the selected line by drawing the piston out slowly. Note volume taken into
cylinder V1, which should be approximately 20 ml for this particular experiment (see
WARNING note below). Wait at least two minutes to allow the gas to come to the
temperature of the cylinder.
9. Isolate the cylinder from the column and the absorption globe and vent the cylinder to
atmospheric pressure. Close after about 10 second.
10. Connect cylinder to absorption globe. The liquid level should not change. If it does
change, briefly open to atmosphere again.

Petroleum University of Technology / Unit Operation Laboratory D-12

D Experiment No.4

Gas
Absorption
Column

11. Wait until the level in the indicator tube is on zero showing that the pressure in the
cylinder is atmosphere.
12. Slowly close the piston to empty the cylinder into the absorption globe. Slowly draw
the piston out again.

Note the level in the indicator tube.

Repeat steps E and F until no significant change in level occurs. Read the indicator tube
marking = V. This represents the volume of the gas sampled.

WARNING:

If the concentration of CO2 in the gas sampled is greater than 8, it is possible to suck liquid
into the cylinder. This will ruin your experiment and lakes time to correct. Under these
circumstances, do not pull the piston out to the end of its travel. Stop it at a particular Mark,
e.g.V1= 20 on the coarse scale, and read the fine scale.

Calculations:

1. CO2 content of gas samples:

From use of Hempl apparatus, volume fraction of CO2 = V2/V1

For ideal gases, volume fraction = mole fraction = Y. Check that the sample taken from the
inlet to the absorption column should give the same value of CO2 fraction as that indicated by
the inlet flow meters.

I.e. V2/V1 = Y1 =F3 / F2 + F3

Petroleum University of Technology / Unit Operation Laboratory D-13

D Experiment No.4

Gas
Absorption
Column

READINGS AT INLET CALCULATIONS

F1(CO2) liters/s F2 (air) liters/s V1 ml V2ml F3/F2+F3 (V2/V1) = Y1

From flow meters From Hempl apparatus

2. Calculation of amount of CO2 absorbed in column from analysis of samples at inlet and
outlet:

From analysis with Hemple apparatus, volume fraction of CO2 in gas stream at inlet =
(V2/V1)1 = Y1.

And at outlet, Y0 = (V2/ V1)0

If Fa is liters/second of CO2 absorbed between top and bottom, then:

[F2 + F1] Y1-[F2 + (F3-Fa)] . Yo = Fa

Fa = (Y1 - Y0) (F2 + F3)/1-Y0 = (Y1- Y0) / (l-Y0) * (total gas inlet flow)

Petroleum University of Technology / Unit Operation Laboratory D-14

D Experiment No.4

Gas
Absorption
Column

NOTE:

Liters/second can be converted to g. moles / second as follows:

Ga = Fa / 22.42 * (av. Column pressure mmHg / 760) * (273/ av. Column temp °C + 273)

Absorbed CO2: ……………………

g.moles/second: …… ………………

The assumption implicitly made here is that the volume flow is not affected by the pressure
drop through the column as this should be small in comparison with atmospheric pressure.

Petroleum University of Technology / Unit Operation Laboratory D-15

D Experiment No.4

Gas
Absorption
Column
Hemple Apparatus for gas analysis

a) Fill with standard reagent to b) Taking gas sample c) Discharging to atmosphere

"0" on scale

Repeat B and C to remove gas from sample lines .then take true sample by further repeating
step B to selected volume V1.

d) Venting to atmosphere e) Charging Hempl f) Withdrawing gas sample

(Balancing pressure) apparatus and taking reading V2

Repeat E and F slowly until V2.

Petroleum University of Technology / Unit Operation Laboratory D-16

E Introduction

Water
Cooling
Tower

The Water Cooling Tower has been designed to give students an appreciation of the
construction, design and operational characteristics of a modern evaporative cooling system.
The unit is also an excellent example of an 'open system' through which two streams of fluid
flow (water and air) and in which there is a mass transfer from one stream to the other.
Convincing energy and mass balances are obtained and students can quickly investigate the
effects of air flow rate, water flow rate, water temperature and cooling loads on the
performance of a cooling tower. They will measure the performance of the cooling tower, and
determine the errors of your sensors and uncertainties of your measurements.

Petroleum University of Technology / Unit Operation Laboratory E-1

E Introduction

Water
Cooling
Tower

Physical Data:

 The load tank contains heaters of 0.5, 1.0 and (1.0+ 0.5= 1.5 KW) heating power.
 Each packed column has dimensions of 150 mm ×150 mm × 600mm high.
 Orifice diameter= 80 mm.
 Orifice constant= 0.0137 Kg1/2.sec-1.m3/2. (mm water)-1/2.
 Energy transferred to water by pump = 0.1 KW.

Packing Data:

A B C
Number of Decks 8 8 8

Number of Plates per Deck 7 10 18

Total Surface Area of

Packing (m2)
0.83 1.19 2.16

Height of Packing (m) 0.48 0.48 0.48

Packing "Density"
(Area/Vol. = m-1)
77 110 200

Petroleum University of Technology / Unit Operation Laboratory E-2

E Introduction

Water
Cooling
Tower

Warnings

1. To prevent scaling problems:

a. Use distilled water for filling this unit.
b. Drain the system after the end of your experiments.
2. Before attempting your experiments, make sure that the depth of the after the water
level in the makeup tank is greater than 50 mm, after the needle valve in the load tank
is closed.
3. The water and air stream temperature must not be allowed to exceed 50 ºC.
4. The air heater must not be switched on, unless the fan damper is open and the fan is
running.
5. The wet bulb reservoirs must be filled with distilled water.
6. Check that:
a. The water flow rate is about 40 gm/sec. when the water control valve is fully
open.
b. The pressure drop across the orifice is about 16 mm H2O when the fan inlet
shutter is fully open.
7. After any water flow rate reduction, wait at least for 10 minutes before collecting the
data.
8. Correct the wet bulb temperature readings for air velocity.
9. For shutting down:
a. Switch off all heaters.
b. After about two minutes switch off all power supplies.
c. Completely drain the load tank.

Petroleum University of Technology / Unit Operation Laboratory E-3

E Introduction

Water
Cooling
Tower

Questions:

1. Investigate the effect of:

a. Air flow rate
b. air temperature and humidity at inlet
c. water flow rate
d. water temperature
e. coding load
f. packing materials

In the performance of a cooling tower.

2. Describe the effect of water flow rate reduction on water level in the load tank.
3. Define the concept of "approach to wet bulb" and describe the relationship between
"approach to wet bulb" and "effectiveness of the tower".
4. Define the following terms:
a. Absolute humidity
b. Relative humidity
c. percentage of saturation

At what condition items b & c are nearly equal together? (Why?)

5. What is a "wet and dry bulb" type hygrometer, and how it works?
6. Describe the effect of air velocity on the indicated wet bulb temperature.
7. Compare the changes in wet and dry bulb temperatures across tower. (give the reasons)

Petroleum University of Technology / Unit Operation Laboratory E-4

E Experiment No.1

Water
Cooling
Tower

Aim: Determination of all "end state" properties of the air and water from charts and tables,
and the application of the steady-flow equation to the selected systems to draw up energy and
mass balances.

Procedure:

1. The water cooling tower should be prepared, started and allowed to stabilize under the
following suggested conditions:
a. orifice differential 1 0 - 1ft mm water
b. water flow rate 30 - 40 gm. sec
c. cooling load 0.5 - 1.5 KW
d. air pre-heat 0.0

2. At regular intervals over a measured period of say 10 minutes, all temperatures and
flow rates should be noted and the mean values entered on the observation sheet.
3. Determine the quantity of makeup water which has been supplied in the above time
interval
4. The observation must be repeated at other water or air flow rates and with another
cooling load.

Calculations:

With the aid of the data obtained, verify the steady flow mass and energy balance equations
for each of the following systems.

Petroleum University of Technology / Unit Operation Laboratory E-5

E Experiment No.1

Water
Cooling
Tower

I)

II )

Petroleum University of Technology / Unit Operation Laboratory E-6

E Experiment No.2

Water
Cooling
Tower

Aim: Effect of cooling load on "Wet Bulb Approach".

Procedure:

1. The water cooling tower should be prepared, started and allowed to stabilize under the
following suggested conditions:
a. Water flow rate 30-40 gm.sec -1
b. Air flow manometer differential 10 - 16 mm water
c. Cooling load 0.0

2. Record the observations in the attached data sheet.

3. While keeping the water and air flows constant, the load should be increased to 0.5 KW,
and when conditions have stabilized, the observations should be repeated.
4. Similar tests should be made with cooling loads of 1.0 and 1.5 KW.
5. The four tests must then be repeated at another constant air flow rate.

Calculations:

1. Plot the "Wet Bulb approach " VS. " cooling load" at different air mass flow rates.

Petroleum University of Technology / Unit Operation Laboratory E-7

E Experiment No.3

Water
Cooling
Tower

Aim: Relation between air velocity and:

a. Wet bulb approach

b. Packing pressure drop

Procedure:

1. The water cooling tower should be prepared with the selected packed column, and set to
stabilize under the following suggested conditions:
a. Water flow rate 30-40 gm.sec -1
b. Air flow manometer differential 16 mm water
c. Cooling load 0.5-1.5 KW

2. Fill the observation sheet with the obtained data.

3. The test should be repeated with three other selected pressure drops
of 10, 4 and 1 mm water at constant water flow rate and cooling load.
4. The test must then be repeated:
a. At another constant load.
b. At another constant water flow rate.
c. Using another packing.

Calculations:

1. Plot the wet bulb approach and packing pressure drop vs. air velocity.
2. Comment upon the obtained results.

Petroleum University of Technology / Unit Operation Laboratory E-8

E Experiment No.4

Water
Cooling
Tower

Aim: Relationship between "Cooling load" and "cooling Range".

Procedure:

1. The water cooling tower should be prepared with the selected packing and set to stabilize
under the following suggested conditions.
a. Water flow rate 30-40 gm.sec -1
b. Air flow manometer differential 16 mm water
c. Cooling load 0.0

2. Record the observation in the attached data sheet.

3. The cooling load should then be increased to 0.5 KW without changing the water and air
flow. After stabilization, the observations must be repeated.
4. The observations should then be made at 1 .0 and 1.5 KW cooling load.
5. The test must then be repeated:
a. At other water flow rate
b. At other air flow rate
c. With pre-heated air
d. With other packings.

Calculations:

1. Plot the water inlet and Outlet temperatures V.S. cooling load. (On the same graph) for
each set of collected data.
2. Show the cooling range and the inlet air wet bulb temperature on each of the above graphs.
3. Discuss about the effect of each variable (e.g. water flow rate, etc ...) on the cooling range.

Petroleum University of Technology / Unit Operation Laboratory E-9

E Experiment No.5

Water
Cooling
Tower

Aim: Investigation of the effect of inlet relative humidity on the performance of the cooling
tower.

Procedure:

1. The water cooling tower should be fitted with the selected column prepared, started and
allowed to stabilize under the following suggested conditions:
a. Water flow rate 25-35 gm.sec -1
b. Air flow manometer differential 10 - 16 mm water
c. Cooling load 0.5-1.5 KW
d. Air preheat 0.0

2. Record the observation in the attached data sheet.

3. The air preheater should then be switched to approximately 0.5 KW, without changes in
the other settings.
4. When conditions have stabilized, the observations should be repeated.
5. The observations should then be repeated at other cooling loads, air flow rates and water
flow rates.

Calculations:

1. With the aid of data obtained, explain the relationship between the inlet relative humidity
and the performance of the tower.

Petroleum University of Technology / Unit Operation Laboratory E-10

E Experiment No.6

Water
Cooling
Tower

Aim: Investigation of the effect of packing density on the performance of the cooling tower.

Procedure:

1. The water cooling tower should be prepared, started and allowed to stabilize under the
fallowing conditions:
a. Water flow rate 25-35 gm.sec -1
b. Air flow manometer differential 10 - 16 mm water
c. Cooling load 0.5-1.5 KW
d. Column installed A

2. Record the observations on the attached data sheet.

3. The observations should be repeated at other loads, water flow rates. (This step also
should be repeated after steps 4 and 5).
4. Column A should then be removed and column B substituted.
5. After preparation and stabilization at the same conditions as above, the observations
should be repeated.
6. Column C should be installed and the observations repeated.

Calculations:

1. Show on a graph, the effect of packing density on the performance of the tower. And give
some reasons for such an effect.

Petroleum University of Technology / Unit Operation Laboratory E-11

F Introduction

Wetted Wall
Absorption
Column

Physical Data:

Column diameter = 25.4 mm

Column height = 825 mm

The liquor wetting rate should be controlled at between 0.4 to 0.1 mls per second per unit
perimeter of the column.

Gas velocity should be controlled in the range of 300-600 cm per second.

NOTE 1:

Use the attached graphs to find Air & Water flow rates.

NOTE 2:

The liquor flow should be instituted first and, when a steady flow rate has been established,
the gas containing the component to be absorbed is introduced into the column. When the gas
rate has been established the apparatus should be operated for a minimum period of 2
minutes. Then sample of the liquor leaving the column should then be taken for analysis.

Warnings

Great care should be exercised when opening the ammonia cylinder, initially this should be
done in the presence of the instructor.

Petroleum University of Technology / Unit Operation Laboratory F-1

F Introduction

Wetted Wall
Absorption
Column

Questions:

1. Describe the concentration profile of Diffusing species in the vicinity of the interface.
2. Define the different resistances to mass transfer during the passage of a substance between
the phases.
3. Explain :
a. Henry's law
b. Lewis & Whitman proposal about the equilibrium condition in the gas absorbtion
process.
4. Describe the Ps/HP criterion for the total mass transfer resistance. What are the
limitations?
5. Explain about the different instruments for Determination of mass transfer coefficients,
when the system is:
a. Gas phase controlled.
b. Liquid-film controlled.
6. Define the "Wetting Rate" in a packed absorption tower. Explain the relationship between
the "Wetting Rate" and the performance of the tower.
7. Write the correlation which can be used to estimate the gas phase mass transfer coefficient
(Kg) in a wetted wall absorption column.

Petroleum University of Technology / Unit Operation Laboratory F-2

F Experiment No.1

Wetted Wall
Absorption
Column

Aim: investigation on wetted wall absorption column.

Procedure:

Fill the water reservoir with de-ionized water.

Switch on the water pump and adjust the water flow rate using valve B until the rotameter
reading corresponds to approximately position 10.0. This water rate must be kept constant
throughout the experiment and occasional adjustment of valve B may be necessary. Ensure
that the water flows evenly over the weir wetting the entire surface of the wall.

When the water flow rate has been established; open valve A very slowly to admit air
through the apparatus. Adjust valve A to give initially a rotameter reading on the tube scale
of 10.0 corresponding to an air rate of 8.0 × 10-2 m3/m and allow the air and water flow rate
to stabilize For five minutes.

Fully open valve C and check that the ammonia pressure regulator tightly closed. Partially
open the valve on the ammonia cylinder and then slowly adjust the pressure regulator to give
a pressure corresponding to a flow rate in excess of the required value. Partially close valve c
to obtain the required flow rate; initially, a rotameter scale reading of 7.5 corresponding to an
ammonia flow rate of 4.0 × 10-3 m3/m. Great care should be exercised when opening the
ammonia cylinder; initially this should be done in the presence of the instructor. Allow steady
state conditions to be established for about three minutes and then take the following readings
and samples.

i. Record liquid flow rate.

ii. Record air flow rate.
iii. Record ammonia flow rate.
iv. Note the temperature of the exit liquid and gas stream.
v. Take two 25.0 ml samples of the exit liquid from the vessel provided and seal the
sample bottle to prevent loss of ammonia.

Petroleum University of Technology / Unit Operation Laboratory F-3

F Experiment No.1

Wetted Wall
Absorption
Column

Repeat the experiment a further seven times to obtain eight sets of results. In each
consecutive experiment increase the air flow rate by 2.0 divisions of the rotameter scale and
adjust the corresponding ammonia flow rate to maintain the ammonia concentration in the
inlet gas stream at about five percent by volume.

Analysis of Samples:

Prepare 500 ml of a 0.25M sulphuric acid solution and place in a burette. Add 20.0 ml of the
liquid from the sample bottle to a clean conical flask followed by a few drops of methyl red
indicator; the liquid in the flask will turn yellow. Titrate this solution with the 0.25M acid
until the solution turns red. From the result estimate the concentration of ammonia in the
exit liquor from the column.

The ammonia gas is absorbed into the water flowing down the wet wall very quickly and
although it farms a polarized ion (NH4+); for the purpose of the chemical analysis
calculations, it can be considered to be converted into ammonium hydroxide. That is

NH3+H2O NH4OH

On titration with sulphuric acid this gives ammonium sulphate.

2NH4OH+H2SO4 (NH4)2SO4

So that, if T ml of 0.25M H2SO4 solution are required to neutralize 20.0 ml of the exit liquor
from the column the concentration of ammonia in the exit liquid is:

Petroleum University of Technology / Unit Operation Laboratory F-4

F Experiment No.1

Wetted Wall
Absorption
Column

Calculations:

1. Calculate the gas phase mass transfer of coefficient (Kg) from each set of experimental
data.
2. Comment upon the obtained results.

Petroleum University of Technology / Unit Operation Laboratory F-5