BRIEF DESCRIPTION OF EXPERIMENTS

Chemical Engineering Laboratory II

C&PE 626
Department of Chemical and Petroleum Engineering
University of Kansas

Spring 2015

List of Experiments
1.

Multi-stage Distillation

2.

Continuous Stirred Tank Experiment

3.

Liquid Level Control System

4.

Transient Heat Transfer

5.

Vapor Liquid Equilibria Measurement

6.

IPA Dehydration and Dehydrogenation Studies in a Tubular Reactor

1) Multi-stage Distillation
A. Background
The separation of mixtures into essentially pure components is of central importance in the
manufacture of chemicals. Much of the equipment in the average chemical plant has the purpose
of purifying raw materials, intermediates, and products by multiphase mass transfer operations.
The laboratory utilizes a 21-stage Oldershaw distillation column that can be operated with
continuous feed or with total reflux.
B. Objectives
To operate a laboratory scale, multi-stage distillation column and to reconcile its performance
with expectations based on the operating variables. You will explore the operating envelope for
the column and to integrate the use of CHEMCAD simulator with the operation of the column in
order to evaluate the performance.
C. Experimental Apparatus
The laboratory utilizes a modified Oldershaw column. It has been equipped with appropriate
sensors and control elements for semi-automatic operation. The column is controlled and data is
acquired using the Camile system.
The reboiler counts as the 1st tray, there are 10 stages between the reboiler and feed, and another
10 stages above the feed for a total of 21 trays. The overall process is as follows: Feed is
pumped at a specified power setting from the blue feed container through an electrical resistance
preheater into the column at stage 11. At the top of the column, the overhead vapor is condensed
in a cooling water condenser. The reflux ratio is set on the Camile, reflux drips directly back
into the column, product drips to a volumetric cylinder for measurement. The reboiler is a 200
mL three necked flask heated by a 470 W electric mantle (note that most of the heat from the
mantle is lost to the atmosphere). The bottoms product can be pumped out of the reboiler
through a water-cooled condenser to the collection point. Liquid samples are analyzed using a
refractometer.
Instrumentation for the column is interfaced with the CAMILE and consists of two pumps (feed
and bottoms), bottoms pressure, several temperature measurements, feed and reboiler heaters,
and reflux ratio.
D. Operation
Starting Out
This initializes the Camile application.
1. Press the <run> button on the menu bar.
2. Press <control key> and the blue <startup> button on the Camile.
3. If you ever have to stop running the column quickly, press <control key> and the red
<emergency shutdown> button on the Camile.

Calibrations
1. Pump Calibration
a. Initially run the pump at 100% power for several minutes to ensure the pump is
properly primed.
b. Calibrate the feed and bottoms pumps by sending the flow to the appropriate
volumetric cylinder.
c. Place a well-labeled copy of your calibration spreadsheet in the Data folder for
use by other groups. Be sure to list units and include plots. Have four equations
listed:
1)
feed power setting given the feed flow rate.
2)
Feed flow rate given the feed power setting.
3)
Bottoms power setting given the bottoms flow rate.
4)
Bottoms flow rate given the bottoms power setting.
d. Check your calibrations by setting a pump output, then comparing your measured
results with the calibration.
e. Use the calibration for estimating flow rates and power settings - during normal
operation you must measure the flow rate used.
2. Temperature Calibration
a. Assume the temperature calibrations are correct.
3. Index of refraction
a. The first group should measure the index of refraction of various mixtures of
methanol and IPA.
1)
Measurements should be made by mass.
2)
Plots must be on a volume% basis. Ideal mixtures are linear only on
a volume% basis.
b. Place a well-labeled copy of your calibration spreadsheet in the Data folder for
use by other groups. Be sure to list units and include plots. Have three equations
listed:
1)
Volume% given the index of refraction.
2)
Mass% given the index of refraction.
3)
Mole% given the index of refraction.
Total Reflux Operation
Once the column is loaded with an appropriate amount of the feed stock, it should not be
necessary to add more stock because all the overhead vapor gets refluxed.
Realize that the relative volatility (VLE information) will govern the compositions of the
distillate and bottoms. Note that during operation, the column will hold roughly 40 mL and the
reboiler will hold roughly 200 mL. If you were to start with 220 mL of IPA and 20 mL of
methanol, the reboiler would likely have no methanol all of which would be in the column.
To the degree that you can depend on the temperatures measurements, you can use these with
Txy data from Chemcad to determine the reboiler and distillate compositions. You can obtain
better accuracy by analyzing samples using the refractometer, but BE WARNED, obtaining
samples during steady-state, total reflux operation will remove a disproportionate amount of the
volatile component and will change the steady state of the system.

Operating guidelines Total Reflux:

1. Press the <run> button on the menu bar.
2. Press <control key> and the blue <startup> button on the Camile. This initializes the
Camile application.
3. If you ever have to stop running the column quickly, press <control key> and the red
<emergency shutdown> button on the Camile.
4. Turn on the water for the condenser.
5. Make sure that the lid on the feed tank is not closed tight to prevent a vacuum there, and
allowing feed to flow to the column.
6. Open the valve on the control column that states, vent while filling column.
7. Load the column with the feed provided at 100% pump power.
8. Close the vent while filling column valve.
9. Turn on the reboiler and set OP to a desired value (OP is in terms of percent of the
maximum wattage of the mantle (i.e., 470 W). The maximum is about 50%. Note that
Camile will shut down the equipment if the flask safety (reboiler heater) temperature
exceeds 500 C. If this happens, fix the problem and use the <control><startup> buttons
to reinitialize the apparatus.
10. Set the reflux ratio by setting the <diverter on> on the Camile to 1 second, and <diverter
off> for 1,000 seconds.
11. Monitor the reboiler, feed-stage, and distillate temperatures during the approach to steady
state. Use these temperatures to estimate compositions. Steady state is attained when the
temperatures, and thus the compositions, are steady. Slowly rising temperatures may
indicate a leak in the apparatus. Record the temperatures every 10 minutes in the
laboratory notebook.
12. Only upon reaching steady state, obtain refractometer data for the bottoms and distillate.
Subtract the composition and volume removed from the total inventory in the column.
13. Dispose of samples in the steel safety can provided.
14. If you need help, ask Jon for assistance.
Operating Guidelines Continuous Distillation:
1. Press the <run> button on the menu bar.
2. Press <control key> and the blue <startup> button on the Camile. This initializes the
Camile application.
3. If you ever have to stop running the column quickly, press <control key> and the red
<emergency shutdown> button on the Camile.
4. Turn on the water for the condenser.
5. Make sure that the lid on the feed tank is not closed tight to prevent a vacuum there, and
allowing feed to flow to the column.
6. Open the valve on the control column that states, vent while filling column.
7. Load the column with the feed provided at 100% pump power.
8. Close the vent while filling column valve.
9. Turn off the feed pump.
10. Turn on the reboiler and set OP to a desired value (OP is in terms of percent of the
maximum wattage of the mantle (i.e., 470 W). The maximum is about 50%. Note that
Camile will shut down the equipment if the flask safety (reboiler heater) temperature

exceeds 500 C. If this happens, fix the problem and use the <control><startup> buttons
to restart the experiment.
11. Set the reflux ratio by setting the <diverter on> and <diverter off> to appropriate times
(<diverter on> plus <diverter off> should total roughly 20 seconds).
a. If you used very long times for on and off, the column would cycle between
two steady states.
b. If you use too short of times, the uncertainty in the times would be sufficiently
great as to make the true reflux ratio unknowable.
12. Wait for the column to heat. When distillate starts to form, activate the feed pump for
operation in the 2 10 ml/min range.
13. Set the feed heater power to obtain the desired feed temperature.
14. Keep track of the distillate flow rate. The bottoms flow rate should be set such that
Feed Flow Distillate Flow = Bottoms Flow. Try to keep the liquid in the reboiler at a
constant level. The bottoms flow may require minor adjustments several times during the
experiment. It is preferable to adjust the bottoms flow instead of the feed flow because
changing the bottoms flow does not change the steady state compositions in the column.
15. Record all changes to the flow rates.
16. Once the reboiler level appears to have stabilized (to some extent), monitor the column
temperatures, and liquid composition while approaching steady state. Steady state is
deemed to have been attained when the temperatures and refractometer readings are fairly
steady. Slowly rising temperatures may indicate a leak in the apparatus.
17. Record in the notebook temperatures and refractometer (composition) data during the
approach to steady state. Record every data available in a data file and in the lab
notebook when steady state is deemed to have been attained.
18. If you need help, ask Jon for assistance.
How long does it take to reach steady state?
If you took samples and recorded temperatures at one-minute intervals, you would find their
values to be almost identical but you would not be at steady state. Use the residence time
to guide you in how often to take measurements. The volume of the system is roughly 240
mL. If your flow is 6 mL/min, then the residence time is 240 mL/ (6 ml/min) = 40 minutes.
Therefore, 20 - 40 minutes between measurements would be more appropriate. As a ballpark
estimate, it will take 3-5 residence times to reach steady state (assuming you do nothing to
upset the approach to steady state).
Other notes
1. During start up, the user needs to monitor the system to ensure that it is behaving as
expected. For example:
Is the feed being heated to the set point temperature (Refer to the section control
loop configurations)?
Is the reboiler liquid level held at a reasonable level? This can be achieved by
small manual changes in the bottoms flow rate.
Is the heating mantle functioning flawlessly?
Is the reflux temperature steady at the set point (Refer to the section control loop
configurations)?

Are the feed stage temperature and other temperatures along the column
approaching expected or set values?
2. When ready to change operating conditions, ask Jon if you require assistance. Some
operating parameters that can be changed are feed compositions (the feed pump will have
to be shut down for a few seconds to change the stock), reflux ratio, feed flow rate, and
reboiler duty.
3. When ready to shut down, <control> <emergency shutdown> buttons.
E. Dos and Donts
1. DO NOT LET THE REBOILER RUN DRY. If the reboiler is close to running dry,
turn off the heater and the bottoms pump.
2. Do not leave the feed heater on for long periods when there is no feed flow (there is no
feed flow during calibration and sampling).
3. Pay attention to your operating parameters - determine what you expect to happen.
Except for some safety items, there are no whistles that will alert you that you are
running the apparatus incorrectly or that the apparatus has a "problem." You are the
operating, you determine if there is a problem, then take appropriate action.
F. Safety
1. Wear safety glasses at all times. Wear gloves when taking samples.
2. In this experiment, methanol and isopropanol are used. Both substances are toxic and
flammable. Review the MSDS sheets for these substances located in the CPE-626 folder
on the world drive. If the chemicals get on you, use the eyewash or shower. In case of
fire, use the fire extinguisher.
3. Do not let the reboiler run dry! If the reboiler is close to running dry, turn off the
heater and the bottoms pump.
4. Do not leave the feed heater on for long periods when there is no feed flow (there is no
feed flow during calibration and sampling).
5. Turn on the hood.
6. Guard against falls, burns, cuts, and other physical hazards.
7. Think of safety in any action you take. If not certain, ask a faculty member before you
act.
8. The experiment is protected with ground fault breakers to help prevent electrocution.
Care should always be taken when combining electricity with water.

methanol MSDS information

Health Hazard Level 1 (on 4 point scale)
Health Hazard Acute And Chronic: Harmful/fatal if ingested/absorbed through skin. Ingestion
of 1 4 oz can cause irreversible injury to nervous system, blindness, death. Cant be made nonpoisonous. Causes eye/respiratory system irritation. May cause skin irritation, defatting.
Harmful if inhaled. May cause internal organ damage. Vapor inhalation/liquid penetration of
skin can cause CNS depression (supple).
Signs/Symptoms Of Overexp:
Inhalation: Nausea, drow, vertigo, FTG, convulsions, unconsciousness, death.

Eye: Burning sensation, tearing, redness, swelling. Conjunctivitis, corneal burns.

Ingestion: Blindness, systemic acidosis, symptoms may be delayed. Medical condition
aggravated by Exposure: personnel with pre-existing CNS disease, skin disorders, impaired liver
or kidney function, or chronic respiratory diseases should avoid exposure.
Emergency/First Aid Proc:
Inhalation: Immediately remove to fresh air. Keep victim quiet. Give air/oxygen and/or CPR.
Eye: Immediately flush with lots of water for at least 15 minutes, opening eyelids.
Skin: Immediately remove contaminated clothing. Wash area well with soap/water.
Ingestion: Symptoms may be delayed. Life threatening. Conscious drink 2 glasses of water.
Induce vomiting. Follow emesis with 2 teaspoons of baking soda in water. Ethanol therapy may
be indicated. In all cases see doctor immediately.
Isopropanol MSDS information
Health Hazard Level 1 (on 4 point scale)
Target Organs: Kidneys, central nervous system.
Potential health affects
Eye: Produces irritation, characterized by a burning sensation, redness, tearing, inflammation,
and possible corneal injury.
Skin: May cause skin sensitization, an allergic reaction, which becomes evident upon reexposure to this material. Prolonged and/or repeated contact may cause defatting of the skin and
dermatitis. May cause irritation with pain and stinging, especially if the skin is abraded.
Ingestion: May cause gastrointestinal irritation with nausea, vomiting and diarrhea. May cause
kidney damage. May cause central nervous system depression, characterized by excitement,
followed by headache, dizziness, drowsiness, and nausea. Advanced stages may cause collapse,
unconsciousness, coma and possible death due to respiratory failure.
Inhalation: Inhalation of high concentrations may cause central nervous system effects
characterized by headache, dizziness, unconsciousness and coma. Inhalation of vapor may cause
respiratory tract irritation. May cause narcotic effects.
Chronic: Prolonged or repeated skin contact may cause defatting and dermatitis. May cause
allergic skin reaction in some individuals.
First Aid
Eyes: Immediately flush eyes with plenty of water for at least 15 minutes, occasionally lifting
the upper and lower lids. Get medical aid immediately.
Skin: Get medical aid if irritation develops or persists. Flush skin with plenty of soap and water.
Ingestion: If victim is conscious and alert, give 2-4 cupfuls of milk or water. Never give
anything by mouth to an unconscious person. Get medical aid immediately. Induce vomiting by
giving one teaspoon of Syrup of Ipecac.
Inhalation: Get medical aid immediately. Remove from exposure to fresh air immediately. If not
breathing, give artificial respiration. If breathing is difficult, give oxygen.
Notes to Physician: Urine acetone test may be helpful in diagnosis.
Antidote: None reported

2) Continuous Stirred Tank Experiment

A. Background
Stirred tanks are used in a variety of situations in chemical plants. In some cases, they may be
used to simply mix several streams or ingredients either in a continuous process or a batch
process. In other cases, the tank may act as a chemical reactor, again in either continuous or
batch processes. Different approaches may be taken for analyzing the transient characteristics of
these tanks depending on the tanks ultimate use. For instance, if the tank is used to mix streams
to form an outlet stream with specified concentration, we may be interested in the system
response as viewed from a process control standpoint (i.e., does this act as a first order or second
order system? Do we need to include dead time?). However, if the tank is to be used as a
reactor, we may wish to determine how closely the tank behaves like a perfectly mixed
continuous stirred tank (CST). If the tank is poorly described by an ideal mixing assumption, we
may wish to model the system as a series of CSTs or other types of reactor models.
B. Objective
To characterize the residence time distribution in a stirred tank.
C. Experimental Apparatus
The apparatus consists of a 40 liter tank equipped with a mechanical stirrer and baffles. The inlet
to the stirred tank runs through a flow meter, which is interfaced with the Camile. The outlet line
from the tank is constructed so that the amount of water in the tank remains roughly constant. A
salt tracer is injected into the tank. The conductivities of the influent and effluent are monitored
at regular time intervals using probes interfaced with the Camile. The frequency of the
mechanical stirrer is also recorded using the Camile. There is also a pressure transducer used as
a level indicator and a thermocouple to measure tank temperature.
D. Operation
Calibration
1. Calibrate the flow meter by removing the hose leading to the tank, then using the
bucket/stopwatch method.
2. The pressure transducer indicating water volume (mass) has been calibrated for you.
Verify the calibration by closing the outlet and adding a known mass of water to the tank.
a. The uncertainty of the mass with the stirrer off is 0.25 kg.
b. Activating the stirrer can cause the indicated mass to increase from 0 to 0.30 kg
above the correct value.
3. You will not calibrate the conductivity probe per se, however, you need to determine the
range of salt concentrations for which the conductivity is linear. Remove the inlet
conductivity probe and use it to measure conductivities of known concentrations of salt
water. Thereafter, use salt concentrations in the tank that are linear with conductivity.
The maximum is not known at this time, but is less than 6 g salt/L. Announce the
maximum value for linearity in the laboratory notebook - make sure this is well labeled
for viewing by future groups.
Two main types of experiments will be used: Step Change, and Pulse

Operating Guidelines: Step Change

1. Fill the tank with tap water.
2. Turn off the incoming water, close the outlet, then add an amount of concentrated salt
solution to the tank.
3. Activate the mechanical stirrer.
4. After the solution is well mixed (about two minutes), quickly open then close the outlet.
This permits the concentration in the outlet (where the conductivity probe is located) to
equal the concentration inside the tank.
5. Activate the logging function of Camile. Logging should be once every 20 - 30 s. Make
the baseline is logged for at least two minutes.
6. Both the inlet and outlet valves are opened. The conductivity of the outlet stream is then
monitored in time. You must come up with a way to ensure that during this starting of the
flow, the tank level varies as little as possible.
Operating Guidelines: Pulse
1. Fill the CST with tap water initially and maintain a steady flow of water through the tank
by opening both the inlet and outlet valves.
2. Activate the mechanical stirrer.
3. Activate the logging function of Camile (once every second). Obtain a two minute
baseline before adding the salt solution. One minute following the introduction of the
salt solution, logging may be decreased to once every 20 - 30 s.
4. Once a steady flow and steady tank level have been achieved, an amount of salt water is
injected into the inlet line of the tank from the attached reservoir. Note that the height of
the injection pipe may be raised or lowered.
E. Analysis
There are numerous ways to analyze mixing. The following is but one method.

0 F C dt M

(2.1)

M C0 V

(2.2)

F C dt
1
C0 V

(2.3)

where:
C = salt concentration (g/l) = constant*conductivity
C0= salt concentration that would be achieved at time zero if mixing were ideal (g/l)
F = flow rate (l/min)
t = time (min)
M = mass of salt introduced to tank (g)
V = tank volume (l)

II
ln C/C0

Slope =

C/C0

extrapolate

tF/V
t F/V

III
C/C0

Back calculated
from
extrapolation

t F/V
Figure 2.1: Procedure for integrating elution profile
I: plot of concentration in dimensionless time
II: plot of log concentration in dimensionless time
Extrapolate for longer periods of time
III: plot of concentration using original data plus extrapolated profile
If your value for F/V is correct, then integrating equation 3 should yield a value of 1. If your
value is not 1, then your value for F/V is incorrect. See Jon if there is a problem.
You are now ready to analyze your experimental data. The experimental response curve (for
example Figure 1-II) can be described by

T F/V

ln

C
tF
F


C0
V
V

Case

Perfect mixing
plug flow
dead space
bypassing
error in F/V
system lag

1
>1
>1
<1
<,>
1
1

(2.4)

F/V

0
>0
0
<0
0
0

Where:

= slope after initial mixing

F/V = system phase shift

effects

NOTE: If you place the wooden meter stick on the flat ring above the drain tube:
V = H*1.6573+1.5775
where:
H = height of water surface (cm)
V = volume (L)
F. Dos and Donts
1. Care should be taken that the initial concentration of salt in the tank (not the
concentration of salt in the solution added to the tank, which will of course be much
higher) does not exceed the level of linearity with conductivity.
2. Do not put salt in the tank without first dissolving it. This will lead to solid salt falling
into the drain, altering the conductivity measurement.
3. The analysis above is just one of many ways of analyzing mixing - find some other ways
from the literature.
4. For the Step Change experiment, the trick will be to make sure that the water level does
not change after the flow is commenced. Think of ways to ensure the water level stays
constant.
G. Safety
1. Wear sturdy shoes suitable for a possibly wet and slippery floor.
2. The experiment is protected with ground fault breakers to help prevent electrocution. Care
should always be taken when combining electricity with water.
H. References:

Holland, C. D., and R. G. Anthony, Fundamentals of Chemical Reaction Engineering, second

ed., Prentice-Hall, Englewood Cliffs, NJ (1979).
Fogler, H.S. Elements of Chemical Reaction Engineering, 2nd Ed., Prentice Hall, Englewood
Cliffs, NJ, 1992). (chapters 13 and 14)

3) Liquid Level Control System

A. Background
Feedback control remains the single most common type of control used in the chemical industry.
Tuning feedback control loops is an important skill for chemical engineers who make careers in
plant operations. Although the theory associated with determining control parameters such as:
1) process gains and time constants
2) gains of various sensors and transducers
3) selection of controller parameters (gain, integral time constant, and derivative time
constant)
are presented in the classroom, it is helpful to obtain practical experience in the activities
necessary to tune a control system. The purpose of this experiment is to provide you with this
practical experience.
B. Objectives
The goal for the spring semester is to gain practical experience in tuning PID controllers and
observing the affects of parameter changes that take the control valve away from being tuned.
C. Experimental Apparatus
Figure 3.1 is a schematic of the apparatus. There are three tanks labeled A, B, and C. A pump
delivers water from a reservoir to a control valve to the tanks. Various shut-off valves enable the
user to send flow to the bottoms or tops of tanks A and/or B. Further, Tanks A and B, and tanks
A and C can be interconnected or isolated using orifice plates. Before you start, verify that the
tanks are connected in the manner you desire. The effluent from the tanks can be constricted
using downstream valves or an orifice plate.
The Camile system provides a convenient PID control capability as well as the data acquisition
capability with which you are already familiar.

D. Operation
Operating Guidelines - Calibration
1. Calibrate the flow meter.
a. Remove all outlets to tank A, which will act as the bucket
A
B
b. Place the PID controller for the valve in manual.
c. Set the "valve closed" position to some value.
d. Send flow to the top of tank A (sending to the top of the tank instead of the
bottom, provides a steady flow).
e. Measure the flow by noting the rate at which the tank fills.
f. Measure a variety of flows to create a trend line.
g. The maximum "valve open" position is 60%, after which the flow is nonlinear.
2. Calibrate the pressure transducer tank levels.
a. Use the outlet valves in conjunction with the pump to fill the tanks to a variety of
levels. Note the strategically located sight glasses.
3. Now it is time to have fun!!!
C
Operating Guidelines - Tuning
From your control book, you will find a variety of tuning methods. One method is described on
p. 8-18 of Perrys:
1. Set the PID controller for the valve to manual.
2. Set the "valve closed" position to some value.
a. Obtain a steady state level.
b. Note that it can take an inordinate amount of time for the level to steady. Open or
Control
close the valve leading
to theValve
pressure transducer to speed the process.
3. When the level is steady, start logging to obtain a two-minute baseline. Use a 20 s
logging interval.
4. Change the "valve closed" positionFlow
and wait for the new steady state.
meter
5. For estimating the various time constants, you will need to know the time at which the 2nd
derivative of height with respect to time is zero the inflection point. You could plot
height with time and eyeball the time of the inflection point - this is not sufficiently
accurate. Instead, plot d(height)/d(time) or [height(t=i+1) height(t=i-1)]/(2t) vs.
time. The time of the inflection point will be at the peak of this plot. The maximum of
the plot is the slope of the tangent at the inflection point.
6. Make a plot of the level vs. time. Include the tangent at the inflection point (from step 5).
7. Mathematically calculate the intercept of the tangent to the baseline. This is .
8. Mathematically calculate the time for the tuning curve to reach a 0.63 change in the level.
This is .
Figure 3.1: Liquid Level Control Apparatus
9.
Ensure
that the
plot site
fromgauges,
step 6 jibes
with the values
not shown are
secondary
drains,
and overflow
lines. obtained mathematically in steps 7
andshows
8.
This schematic
the physical tank locations relative to each other.
10.
Calculate
P, i, andthat
d from
8-3 ofofPerrys.
For your report, it is suggested
you table
omit parts
the above diagram not used
Operating Guidelines - Changing Set points
1. Set the PID controller to automatic.
2. Set the set point to the initial value of the level used during the tuning procedure.
3. Let the level steady.
4. Log using 10 - 20 s intervals. Obtain a baseline.

5.
6.
7.
8.

Change the Setpoint.

Surf the net for a while.
Plot your results.
Perform steps 2-7 using P, I, or D values that are larger or smaller than the tuned values.

Operating Guidelines - Other

1. You can flow from one tank to another using a straight PID controller, or as a master
slave.
2. You can provide upsets to the inlet pressure
3. You can provide upsets by adding water to the top of one of the tanks.
4. You can provide upsets by draining the tank from the bottom for a short period of
time.
5. Use your imagination.
E. Safety
1. Wear sturdy shoes suitable for a possibly wet and slippery floor.
2. The experiment is protected with ground fault breakers to help prevent electrocution.
Care should always be taken when combining electricity with water.
F. Dos and Donts
If you set a valve position and then merely wait till steady state is reached until started a run, you
will waste 30 100 minutes of valuable time. Instead, help speed the approach to the initial
steady state by opening secondary drains or closing primary drains. For example, say you have
the valve open at 10% leading to tank A, and you are waiting for the initial steady state.
1. Look at the plot of level vs. time on Camile. If you see the level is going down at the rate
of about 1.0 inches in 5 minutes.
a. This means the steady state is at a lower level than the present level.
b. Open the drain that is connected to the line leading from the bottom of the tank to
the manometer to lower the level 4 inches.
2. Check the plot of level vs. time again. This time you see that the level goes down 0.5
inches in 5 minutes.
a. This means that the steady state is at a lower level, but that the tank is closer to
steady state than it was previously.
b. Open the drain again, maybe this time lowering the level 1 inch.
3. Check the plot of level vs. time again, and proceed as appropriate. You may stop when
you feel you are sufficiently close to steady state to obtain a good run.
Note that different flow configurations and outlet valves will change the time constant of the
approach to steady state. Use the trial and error method to estimate how much to raise or lower
the tank level in your approach to steady state.

F. References
1. Ogunnaike, B. A. and W. H. Ray, Process Dynamics, Modeling and Control, Oxford
University Press, 1994.
2. Perry, J.H., Editor, Chemical Engineers Handbook, 8th Edition, McGraw Hill Book
Company, pp. 8: 18-19 (2008).

4) Transient Heat Transfer

A. Background
The non-steady-state heating and cooling of process tanks is an important task in many areas of
chemical engineering. The experimental apparatus permits the cooling of a hot water tank using
a jacket or a coil through which cooling water flows.
B. Objectives
To determine the functionality of coolant flow rate, stirrer speed, and baffles on transient heat
transfer coefficients.
C. Experimental Apparatus
The apparatus consists of a stirred tank fitted with a cooling jacket and with internal cooling
coils. Measured variables include coolant water flow rate, tank temperature, and inlet and outlet
coolant temperatures. A baffle is also available.
D. Operation
Operating Guidelines - Calibration
1.
The flow has been calibrated previously; however, perform a check of the flow
calibration. Be sure to record the check in your notebook and in your report.
2.
Calibrate the stirrer speed using the manual tachometer.
a. Create a spreadsheet to calculate rpm given dial indication and vice versa
b. Place a well-labeled copy of this spreadsheet in the Data folder for use by other
groups.
Operating Guidelines - Experiments
1. Fill a beaker with roughly 1.8 L of hot water from the tap. Further heat the water in the
microwave oven to about 70 - 80C.
2. While the water for the tank is heating, have cooling water flowing to the jacket or coil
heat exchanger.
a. This is to prevent cooling of the inlet during the experiment.
3. Begin logging using 20 s intervals.
4. Momentarily stop cooling water flow.
a. This is to keep the tank water as hot as possible until the apparatus is completely
prepared.
5. Weigh the hot water, then add to the tank.
6. Install the tank cover
7. Position the tank thermister about 1 cm above the bottom of the tank.
8. Set the stirrer at the desired rotational speed.
9. Restart the cooling water flow.
10. Start heating the next beaker of hot water.
11. Stop the experiment when the difference between the inlet and outlet temperatures is
around 2 - 3 C.
12. Analyze your data immediately.

E. Dos and Donts

Do not allow the flow rate to exceed 50 g/s. The plastic bearings in the flow meter may be
damaged.
F. References:
Experimental Manual for the Armfield HT43X Heat Exchanger
G. Safety
1. The experiment is protected with ground fault breakers to help prevent electrocution.
Care should always be taken when combining electricity with water.

5) Vapor Liquid Equilibria

A. Background
Vapor Liquid Equilibria is useful in a variety of chemical engineering applications - from
absorption to distillation and condensation.
B. Objective
In this experiment you will gather data for VLE for a binary system using an Othmer Still. You
will sample condensed vapor in equilibrium with a liquid and measure its composition using a
refractometer. Thus, a T-x-y plot can be constructed.
C. Experimental Apparatus:
The Othmer Still is designed to facilitate the collection of vapor and liquid samples in
equilibrium. It is a batch still, with a condenser and total reflux. Heat is provided by an
immersed resistance heater. The temperature of the vapor above the boiling liquid is measured
by a thermocouple probe or thermometer. The returning condensed vapor is sampled, its
composition determined by measuring its index of refraction. While it is possible to sample the
liquid phase, this is not desirable because unknown quantities of vapor would simultaneously
escape. Instead, the composition of the liquid is calculated by keeping an inventory of the
masses added and removed from the system.
D. Operation:
Operating Guidelines Refractometer
Startup

The refractometer should already have been on for 30 minutes with a setpoint
temperature of 20C
If the refractometer is not already on, turn the instrument using the power switch on
the back. Wait for 30 minutes before proceeding to the next step
If the temperature is other than 20C, press <SETUP> and scroll the temperature
setpoint to 20C

One Point Calibration do this at the start of lab

(do not confuse this with the index of refraction calibration below)
Press <CALIBRATE>
Clean the prism using a Chemwipe
Press <CALIBRATE> again
Press <MODE> until the display shows the current mode is Index-TC
Use a squeeze pipette to deliver enough RO water to cover the prism, and then
close the cover
Press <CALIBRATE>
When the temperature stabilizes, the reported value should be 1.33299 +/- 0.0005

Clean the prism using a Chemwipe

Press <SETUP> The machine should show index
It should not show index TC.
If the machine does not show index, press <MODE> until it does show index.
The Refractometer is now ready for use.
Refractometer use
Clean the prism using a Chemwipe
Use a squeeze pipette to deliver enough RO water to cover the prism, and then
close the cover
Press <READ>
Operating Guidelines - Index of Refraction Calibration
1. The first group should measure the index of refraction of various mixtures of methanol
and IPA.
a. Measurements must be made by mass.
b. Plots must be on a volume% basis. Ideal mixtures are linear only on a volume%
basis.
c. Place a well-labeled copy of your calibration spreadsheet in the Data folder for
use by other groups. Be sure to list units and include plots. Have three equations
listed:
1)
Volume% given the index of refraction.
2)
Mass% given the index of refraction.
3)
Mole% given the index of refraction.
Operating Guidelines - Vapor Liquid Equilibria
1. Turn on the cooling water.
2. Tare a beaker with pure liquid of your first component.
a. Add sufficient liquid to the still to cover the heating elements.
b. Keep an inventory of the masses added to the still.
3. Close the inlet and turn on the heater. Do not use greater than 30% power without
permission.
4. Soon, vapor will begin to condense. Monitor the temperature for approach to steady
state. Estimate the rate of condensation by timing how long is required to fill the arm
containing the condensate.
a. The very first time, after the arm fills with liquid, turn off the heater, let the
temperature cool for a minute.
b. Measure the mass of liquid in the arm.
c. Calculate using the density and mass, the volume of liquid in the arm.
d. The rate of condensation is important to know, this gives you an idea of the
residence time of the vapor passing through the condensate arm. As a ballpark
estimate, it will take 3-5 residence times for steady state to be attained.
5. When steady state is attained, turn off the heater and let the still cool for a minute or so.
6. Remove a sample using a tarred vial.
a. Keep the sample sealed until ready for analysis.
b. Obtain the mass.

c. From the index of refraction, obtain the volume%, mass%, and mol%.
7. Determine the moles of each component in the arm, then by subtracting this from the
total moles, determine the moles of each component in the still.
8. Subtract out the sample removed from the amount of each component in the entire
inventory.
9. Add enough of the second component to the still to increase its percentage by about 10%,
update the inventory, and continue with steps 3 - 9.
10. Stop when you have roughly a 50% mixture. Drain the still and start from the other side
of the Txy diagram.
11. Important note: Any errors you make to the inventory will be additive to previous errors.
Waste Materials: At the end of the experiment you will have a fair amount of waste. Pour these
into the steel safety can provided.
E. Safety
1. You must always use safety gloves when handling any liquid samples.
2. Breakage be careful. Do not try to pick up the still. Dont move heavy hard objects
near it.
3. Do not let the still run dry.
4. Do not plug in the heater until fluid covers the coils. If you do, the coils will
instantaneously turn red hot and melt.
5. Make sure you know where the fire extinguisher is and how to use it.
6. Note the location of the safety shower.
7. Avoid breathing the vapors of solvents.
8. Review the MSDS sheets for the substances used see Jon if you cannot find this
information
9. The experiment is protected with ground fault breakers to help prevent electrocution.
Care should always be taken when combining electricity with water.
VLE data for combinations of chemicals: It is interesting to vary the ending group of one of
the chemicals used to see the effect on your Txy diagram. For example
Water - methanol
Water - ethanol
Water - 1-propanol
Or
Methanol 1-propanol
Methanol 2-propanol
Etc.
Figure that you have time to do a maximum of two to three sets of chemicals. You can also
coordinate with groups in other lab sections to get more sets of chemicals
On the following pages you can see some possibilities. Note that not all chemicals form
solutions (for example, you wouldnt want to use butanol-water as one of your combinations)

In order to compare two liquids in the same mixture, for example:

water-methanol, water-ethanol, or water-isopropanol,
IR = .01 volume fraction resolution = 0.01
IR = .02 volume fraction resolution = 0.005
IR = .04 volume fraction resolution = 0.0025
etc.
The smallest acceptable resolution is about 0.01
Ideas for chemicals in which the ending group varies in a regular manner:

Methanol
BP = 65 C
IR = 1.3314

ethanol
BP = 78 C
IR=1.3616

1-propanol
BP = 97 C
IR=1.387

1-butanol
BP = 118 C
IR=1.3993

1-butanol
BP = 97 C
IR=1.387

2-butanol
BP = 118 C
IR=1.3993

1-propanol
BP = 97 C
IR=1.387

2-propanol
BP = 82 C
IR=1.3776

methyl acetate
BP = 57 C
IR=1.361

Ethyl acetate
BP = 77 C
IR=1.372

n-propyl acetate
BP = 102 C
IR=1.384

n-butyl acetate
BP = 127
IR=1.3941

methyl acetate
BP = 57 C
IR=1.361

2-butanone
BP = 80 C
IR=1.3788

2-butanol
BP = 118 C
IR=1.3993

acetone
BP = 57 C
IR=1.359

2-butanone
BP = 80 C
IR=1.3788

acetone
BP = 57 C
IR=1.359

2-propanol
BP = 82 C
IR=1.3776

water
BP = 100 C
IR=1.333

H2O

6) IPA Dehydration and Dehydrogenation Studies in a Tubular Reactor

A. Background
It is generally acknowledged that tubular reactions are the most fascinating subject in chemical
engineering, surpassing not only steady state heat transfer, but also vapor liquid Equilibria.
B. Objective
To investigate the dehydration and dehydrogenation of isopropanol (IPA) in a continuous flow,
tubular reactor, IPA dehydrates to form propylene and dehydrogenates to form acetone. You will
determine reaction rate constants and activation energies for the two reactions.
C. Experimental Apparatus
Helium gas at approximately 60 psig is passed through a set of traps to remove traces of oxygen
and moisture. The Helium is bubbled through a reservoir of IPA cooled by a bath, saturating the
helium with IPA. Downstream of the bubbler, the pressure is measured. The Helium-IPA
mixture can either be directed to the reactor or directly to a gas chromatograph for analysis.
The stainless steel tubular reactor has a 3/8 ID and is equipped with a thermocouple embedded
under the catalyst bed. The reactor is wrapped with a heating coil to adjust the catalyst
temperature.
Flow is measured downstream using a bubble column.
D. Operation
Operating Guidelines - Calibration
1. Connect the pressure transducer to a pressure gauge (in the cabinet below) and to the
helium cylinder leading to the reactor (do not touch the cylinder for the GC).
2. Calibrate the pressure transducer from 0 to 10 psig.
Operating Guidelines - blank runs
The purpose of conducting blank runs is to limit reactions on the reactor walls during your
regular runs. At higher temperatures, the walls of the reactor catalyze the reaction, making
analysis of a catalyst impossible.
1. Verify that the reactor is free of catalyst.
2. During an experiment, set the flow at roughly 80 sccm
3. Set the temperature to 100C.
4. Run the GC repeatedly until you have three consecutive chromatograms with peak areas
that are within 1% of each other.
5. Calculate the reaction rate, leaving V as a variable (see eq. 6.5).
6. Increment the temperature by 50C. Repeat steps 4-6 through 300C.
7. Use the data to obtain the pre-Arrhenius factor and activation energy.
8. You will use the results of step (7) to determine the validity of rate constants for the
catalyzed reactions. A valid rate constant for a catalyzed run requires less than 5% of the
reaction to be caused by the wall.

Note: There is frequently a bottleneck caused by inattention to the GC. Do not less the GC
rest.
Operating Guidelines - Experiments
1. Load the reactor from the top with between 0.5 and 2.0 grams of catalyst. The catalyst is
held in place within the reactor by a screen fixed approximately 3 from the bottom.
2. Set the temperature of the coolant bath between -10 and 15 C. Temperatures at the low
end can require an hour of waiting - contact the laboratory supervisor prior to the lab to
have the coolant bath ready for you at the lower temperatures.
a. Do not use bath temperatures higher than 15C because the Gas Chromatograph
response is not linear at higher concentrations.
9. During an experiment, flow can be set between roughly 20-120 sccm and temperature can
be set between 25 and the upper temperature determined during the blank run, in roughly
25C increments.
10. Once steady temperature has been achieved (in roughly 10-30 minutes following each
setting), the exit stream from the reactor is fed into a gas chromatograph.
11. Each sampling takes 10 minutes to be analyzed by the GC.
12. Run the GC repeatedly until you have three consecutive chromatograms with peak areas
that are within 1% of each other.
Table 6.1 provides the GC settings and sample elution times.
Table 6.1: HP 5890 Series 2 Gas Chromatograph Settings
Injector
Temperature 160 C
Column
Temperature 160 C
Detector
Temperature 160 C
Column
Pressure
40 psig
Theory
The reaction of Isopropanol follows two possible routes:
C3H7OH

C3H6O + H2
C3H7OH

C3H6
+ H2O

(6.1)
(6.2)

Follow the development of the plug flow reactor in Example 4-4 of Fogler (1986). Similar to the
example, for each of the above reactions we have two products:
A B+C
(6.3)
Initially, we will consider the two reactions (6.1 and 6.2) to be a single reaction. Our design
equation is:
x dx
V F A0
0 r
A
(6.4)

Note that V is the volume of the catalyst. For our purposes, V is calculated independently:

bulk

(6.5)
where m is the mass of the catalyst and bulk is the bulk density - the density based on both the
catalyst and the void space. You need to measure both these values prior to the experiment.
The rate law is given as:

rA k C A

(6.6)

Be careful as CA is often misunderstood. CA is the concentration of the reactant at the

temperature and pressure of the reactor.
Realizing that this reaction involves a change in moles, We must introduce .
=yIPA,0 = yipa,0(1 + 1 1) = yipa,0

(6.7)

Isopropanol is assumed to reach saturation in the bubbler prior to the reactor. Use Perrys (Page
2-59, Table 2.8, Entry No. 282) to create a correlation for isopropanol vapor pressure in psia
between -10 and 15C.
You will need to check your results to verify that the expected mole fraction of IPA is the actual
mole fraction. Remember that Camile reports Preact in psig.
y IPA, 0

where:
xtotal

y acet y prop
xtotal (1 y acet y prop )

(6.8)

y acet y prop
y acet y prop y IPA

(6.9)

note that:
x acet
x acet

y acet

y acet
y prop y IPA

(6.10)

y prop
y acet y prop y IPA

(6.11)

Solving equation (6.4), we arrive at:

k total

FA0
1
xtotal
(1 ) ln
V C A0
1 xtotal

(6.12)

It is noted that the volumetric flow rate, v0 is at reactor temperature and pressure, but the flow is
actually measured upstream of the reactor at STP (1 atm, 0C) before the addition of IPA. Any
complexity is due to the density and therefore the concentration and volumetric flow rate varying
with temperature and pressure till the IPA reaches the reactor.
FIPA, 0
Treact
1atm
v0 v measured (1 y IPA,0 )

C IPA,0
298.15K ( Preact Pamb)
(6.13)
Finally, we end up with:
k total v 0

bulk
1
y A0 xtotal
(1 y A0 ) ln
m
1 xtotal

(6.14)

Using the GC peak areas obtained for each compound, the IPA conversion can be
calculated at each temperature setting. The recorder provides peak areas based on the thermal
conductivities of the gases flowing by the gas chromatograph thermal conductivity conductor. A
given mole fraction of some gas has its own conductivity. Thus, the peak areas must be divided
by a thermal response factor.
Areacorr = Arearecorder/thermal response factor
yield acet

yield prop

(6.15)

y acet
y acet y prop

(6.16)

y prop
y acet y prop

(6.17)

Finally, to obtain the individual rate constants,

kprop = ktotal * yieldprop
kacet = ktotal * yieldacet
Table 6.2: Peak Characteristics
Thermal
Elution
Response
Chemical
Time (min) Factor
Propylene
1
*****
Water
2
N/A
Acetone
6
*****
Isopropano 7
*****
l

(6.18)
(6.19)

D. Some issues that may be addressed

1. How does IPA conversion vary with temperature? Are there noticeable transitions from
intrinsic kinetic control to mass-transfer control?
2. How do the propylene and acetone yields vary with temperature?
3. How do product selectivities change using a Pt/y-Al2O3 catalyst instead of a Pt/C
catalyst?
4. How can you decrease external mass transfer resistance?
5. How can you decrease internal mass transfer resistance?
E. Dos and Donts
1. The reactor thermocouple has been calibrated. DO NOT loosen or remove this
thermocouple for calibration purposes. If the thermocouple is loosened or its insertion
depth adjusted, you will obtain poor reactor temperature control and poor reproducibility
of your results.
2. The reactor bypass stream should only be used initially to verify the IPA concentration in
the helium stream entering the reactor. The bypass stream may be shut off after it is
sampled and analyzed. Following this, the Helium/IPA stream is directed to the reactor
till the end of the experiment.
3. Always note the pressure. You cannot perform your calculations without knowing the
pressure of the reactor.
4. Have your spreadsheet set up before you come into the lab. You must perform
calculations as soon as the measurements are taken.
F. References
M. Berlowitz and H. H. Knug, Catalytic Decomposition of 2-Propanol on Single-Crystal
Surfaces of ZnO. J. Am.. Chem. Soc., vol 12, p108, (1986)
J.M., Cunningham and Nunan, J., Surface Reactions and Catalysis of Alcohol Vapor/3d
Transition Metal Oxide Interfaces at T 475 K. Part I. Dehydration and Dehydrogenation of
Isopropanol over V205 and V203 , Can.J.Chem., vol 62, pg 785, (1984)
Perry, J.H., Editor, Chemical Engineers Handbook, 8th Edition, McGraw Hill Book Company,
pp. 2-59 (2008).

G. Safety
1. In this experiment, compressed air and helium are used. If the tubing is improperly
connected, the pressure will cause the tubing to disconnect from its fitting. The primary
danger is from being hit in the eye with this tubing. It is essential that safety glasses be
worn to prevent this danger.

2. In this experiment, isopropanol is used. Isopropanol is both TOXIC AND

FLAMMABLE. Review the MSDS sheets located in the CPE-626 folder on the world
drive. If the chemicals get on you, use the eyewash or shower. In case of fire, use the
fire extinguisher.
3. Be sure the lab ventilation system is operating.
Isopropanol MSDS information
Target Organs: Kidneys, central nervous system.
Potential health affects
Eye: Produces irritation, characterized by a burning sensation, redness, tearing, inflammation,
and possible corneal injury.
Skin: May cause skin sensitization, an allergic reaction, which becomes evident upon reexposure to this material. Prolonged and/or repeated contact may cause defatting of the skin and
dermatitis. May cause irritation with pain and stinging, especially if the skin is abraded.
Ingestion: May cause gastrointestinal irritation with nausea, vomiting and diarrhea. May cause
kidney damage. May cause central nervous system depression, characterized by excitement,
followed by headache, dizziness, drowsiness, and nausea. Advanced stages may cause collapse,
unconsciousness, coma and possible death due to respiratory failure.
Inhalation: Inhalation of high concentrations may cause central nervous system effects
characterized by headache, dizziness, unconsciousness and coma. Inhalation of vapor may cause
respiratory tract irritation. May cause narcotic effects.
Chronic: Prolonged or repeated skin contact may cause defatting and dermatitis. May cause
allergic skin reaction in some individuals.
First Aid
Eyes: Immediately flush eyes with plenty of water for at least 15 minutes, occasionally lifting
the upper and lower lids. Get medical aid immediately.
Skin: Get medical aid if irritation develops or persists. Flush skin with plenty of soap and water.
Ingestion: If victim is conscious and alert, give 2-4 cupfuls of milk or water. Never give
anything by mouth to an unconscious person. Get medical aid immediately. Induce vomiting by
giving one teaspoon of Syrup of Ipecac.
Inhalation: Get medical aid immediately. Remove from exposure to fresh air immediately. If not
breathing, give artificial respiration. If breathing is difficult, give oxygen.
Notes to Physician: Urine acetone test may be helpful in diagnosis.
Antidote: None reported