Ch.E. 327 Chemical Engineering Laboratory (Writing Enriched)

ChE 327 Chemical Engineering Laboratory 1
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Ch.E. 327
Chemical Engineering Laboratory
(writing enriched)
Manual
Widener University
Department of Chemical Engineering
Prof. C. R. Nippert
Fall 2010
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Table of Contents
General Information and Instructions....................................................................................3
Objectives of the Course........................................................................................................................3
Safety......................................................................................................................................................4
Schedules and Duties..............................................................................................................................5
Data Acquisition and Control.................................................................................................8
Data Acquisition and Control with OptoLCSX™ and Factory Floor™...............................................8
Procedure for Using Factory Floor™ Software.....................................................................................9
Statistical Methods in Data Analysis....................................................................................11
Lab Reports............................................................................................................................16
Experiments............................................................................................................................19
1. Measurement of Viscosity................................................................................................................21
2. Friction Loss in Pipes and Fittings...................................................................................................26
3. Transient Response of Two Interacting Tanks................................................................................29
4. Level Control of Tanks....................................................................................................................33
5. Frequency Response of a Control System.......................................................................................37
8. Heat Conduction in Solids................................................................................................................38
9.Unsteady State Heat Transfer............................................................................................................42
10. Film and Dropwise Condensation..................................................................................................46
12. Tray Column Efficiency, Technovate Column.............................................................................50
13. Batch Distillation, Constant Overhead Composition, Technovate Column.................................56
14. Batch Distillation at Constant Liquid Rate, Technovate Column................................................61
15. Batch Distillation at Constant Reflux, Oldershaw Column..........................................................63
16. Absorption in a Packed Column....................................................................................................66
18. Mass Transfer in an Agitated Tank................................................................................................72
19. Fluidization.....................................................................................................................................74
20. Filtration.........................................................................................................................................76
Appendices........................................................................................................................80
Startup and Operation Procedure for the Technovate Still................................................81
Note: Many portions of this text are revisions of earlier versions and are so noted. The
manuscript is in the form of an MS Word document for easy revision. It will be updated
each semester. Please forward comments and potential corrections to the lab instructor.
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General Information and Instructions
Objectives of the Course
1. To be able to use practical, problem solving methods based on use your

theoretical knowledge of transport phenomena, data analysis, mass-transfer
operations, and thermodynamics.
2. To be able to understand the capabilities and accuracy of many common methods

of measurement of process variables, particularly temperature, pressure, flow
rate, and composition of data by computer. To demonstrate that understanding
with appropriate error analysis.
3. To be able to plan and execute experiments, which students will demonstrate by

performing them.
4. To be able to successfully and cooperatively work with others, as demonstrated

by active participation during lab periods and in meetings.
5. To be able to analyze data, and write reports on time as demonstrated by the

completion of laboratory reports.
Note: Some of the experiments are deliberately NOT “cook book” (i.e. with detailed step
by step instructions”. For reasons of safety and economy (some equipment is expensive),
some experiments have detailed procedures. As an engineer, you must learn how to
approach experiments and develop operating procedures yourself. Finally, the manual is
NOT intended to provide all the theoretical information you may need for an experiment.
Use the reference list to acquire the background you need. For many of the
experiments, it will be part of your task to establish the details of the operating
procedure (much as would happen in the development of a new process). Before
performing any experiment, you should review the materials in the appropriate course
text.
Rev. 8/5/02 CRN, rev 7/31/10
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Safety
1. Accidents
Any accident that results in injury to a person or damage to property (yours or
Widener’s), no matter how minor, must be reported to your instructor as soon as
possible. First aid materials are available in the laboratory and the machine shop.
2. Eye protection
Eye protection shall be worn at all times in the laboratory when experimental
work is being performed that involves the handling of hazardous materials that
can splash or dusty powders. Failure to observe this rule will result in dismissal
for the remainder of the class period. Normal eyeglasses are NOT acceptable.
(OSHA 3151 revised 2000, p. 8)
3. Rubber gloves
Rubber gloves are to be worn when handling toxic or corrosive materials
4. Clothing
Laboratory coats or old, snug fitting clothes are the preferred form of dress in the
laboratory. Loose fitting clothes, open sleeves and loose jewelry may not be
worn. Open-toed footwear and bare feet are prohibited. Widener is not
responsible for damage to clothing or shoes.
5. Smoking, eating and drinking

Smoking, eating and drinking are not permitted in the laboratories at any time.
Chewing gum is prohibited when working with volatile materials.
6. Horseplay
Horseplay is dangerous in a laboratory environment and will not be tolerated.
Horseplay will result in instant dismissal.
6. Material Safety Data Sheets

Material Safety Data Sheets (MSDS) for materials used in the experiments are
available in the Chemical Engineering Office and in the cabvinet of textbooks by
the computer for the distillation column. Group leaders should read them.
7. General Safety and Waste

A copy of the Chemical Engineering Department Hygene Plan is kept with the
MSDS sheets. Students needing information on waste disposal or more detailed
safety information should become familiar with the procedures.
Rev. 8/11/02 rev 7/30/10
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Schedules and Duties
Your instructor will prepare a schedule of experiments and organize the class into
groups early in the semester.
Each experiment follows a schedule similar to the one outlined below:
1. A preliminary meeting normally held before the lab period in which the
experiment is to be performed. At this time, the instructor and team will discuss
the objectives of the experiment and theoretical background. All members of the
team must attend this meeting.
2. In general, you will need one or two laboratory periods to perform the
experiment. Prior to the start of the first laboratory period, the team leader
submits a brief (2-5 page) preliminary report. The preliminary report outlines the
duties of each team member and any setup work either the laboratory instructor or
the laboratory technician must perform before the start of the experiment. No set
up work will be performed without a written request from the team submitted at
least 24 hours before the experiment.
3. Laboratory equipment can be dangerous if you are unprepared or don't know
what you are doing. Unprepared teams may be removed from the lab. Owing to
scheduling problems, make up labs may not be possible.
4. Many of the experiments have a Virtual Laboratory component. This component
is used to familiarize you with the operation of the equipment and interpretation
of data. You will be issued an id and password at the beginning of the semester.
The Virtual Lab allows a history of you woprk to be available to the instructor.
You must perform the Virtual Laboratory componente BEFORE performing the
associated laboratory experiment. Failure to complete the module will prevent
you from being admitted to the laboratory. This policy is strictly enforced with
the distillation column for safet resaons.
5. After the first week of an experiment, the team meets with the lab instructor with
their preliminary calculations. The purpose of this meeting is to review your
calculations. If you complete the experiment in the first week, you must come
in the second week and duplicate your results unless you get permission from
the instructor.
6. The first draft of the final report (~8-10 pages text, double spaced) is due one
week after the last scheduled lab period for that experiment. Generally, only
one report, by the team leader is required. Generally, the instructor will return
reports on the next day for final revision. Because of the need for prompt
revisions, extensions for the first draft are rarely given. Unexcused late reports
may earn a grade of "F".
7. Students are to turn in revisions within one week or the author may receive a
grade of "F" for the lab. Be sure to turn in your original marked first draft when
turning in your second report. Lab experiment schedules follow a pattern shown
below. Expect your team to submit a written document to the laboratory
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instructor. With the approval of the instructor, the team may present the last lab
report orally on the last scheduled laboratory day.
Sample ChE Lab Schedule (your acutal schedule

will be issued by the instructor)
Event
Report Report Revised 2nd draft

Experiment (1st draft) Returned Report returned
1
2
3
4
5
6
k 7
e
e
W8
9
10
11
12
13
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Experiment 1 Experiment 2 Experiment 3

Experiment 4 Experiment 5 Experiment 6
Duties of the Team Leader

1. Familiarize yourself with the theory and analytical aspects of the laboratory prior
to discussion of the laboratory, reviewing course material where necessary.
2. Prepare the preliminary report.
3. Coordinate with the instructor and laboratory technician to ensure the proper
resources are ready for the experiment.
4. Assign duties to individual team members.
5. Report any violation of laboratory policies and accidents to the lab

instructor.
6. Ensure the general success of the laboratory experiment.
7. Attend all classes and meetings.
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8. Coordinate the necessary calculations and the writing of the final report and
provide a copy to the instructor ON TIME.
Duties of the Other Team Members

1. Familiarize yourself with the theory and analytical aspects of the laboratory prior
to discussion of the laboratory, reviewing course material where necessary.
2. Perform duties assigned by the team leader.
3. Report any violation of laboratory policies and accidents to the lab instructor.
4. Ensure the general success of the laboratory experiment.
5. Attend all classes and meetings.
6. Assist the team leader with the calculations.
Grades
Grades will be assigned for both the report and the lab itself. Absence from the lab or
prelab will result in a grade of “F” for that period. Grades will be based on
Performance in lab 50%
Reports 50%
Lab performance will be graded on leadership, understanding of the experiment, ability

to use the equipment, degree of supervision required by the instructor. Missed labs
cannot be made up
Rev. 8/11/02 CRN

Rev 8/30/10 CRN
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Data Acquisition and Control

Data Acquisition and Control with OptoLCSX™ and Factory Floor™
Many of the laboratory experiments are interfaced to Opto22 SNAP LCSX

programmable logic controllers (PLCs) through computers running Factory Floor
software. The SNAP LCSX is an “industrial strength” PLC (programmable logic
controller) that can function even when disconnected from the computer. It is hard wired
to an OPTO22 Brainboard™. This configuration allows control rapidly of complex
systems. This is a brief discussion of the system and its operation.
Opto22 Hardware - Basic Configuration with Computer Control:
1. Signal input/output (Analog I/O)

Analog signals (that is, a signal such as voltage that is a continuous function
determined by the measured variable) are brought in from the process terminals
on an input/output (I/O) board. These signals could be voltages or amperages
that are often proportional to force, speed, humidity, flow rate, etc. Sometimes,
however, the signal has a nonlinear relationship to one of those variables (signals
from many flow meters are proportional to the square of the flow, for example).
In addition, some terminals can send analog signals on command from the PLC
or human operator.
In certain cases, where it is desired to send a signal over a long distance, the
analog data are in the form of a current (4 mA = 0, 20 mA = full scale).
Up to 16 inputs or outputs can be handled by the boards in our systems.
2. Signal conditioning
Each set of input terminals is connected to a plug-in signal-conditioning module
that converts analog signals to digital numbers. The conditioner may also convert
data to be proportional to the process variable. For example, it may take the
square root of a voltage from a flow meter to give a conditioned signal that is
proportional to the flow rate. Alternatively, it may amplify a very low voltage
from a thermocouple and fit the result to a table of temperature versus emf to give
a signal proportional to temperature.
3. OptoLCSX
The OPTO LCSX is a programmable logic controller for the Brain Board. It runs
a program downloaded from the computer. It houses PID controllers (as
software), monitors inputs from the brain board and communicates to the
computer. Because it is a PLC, it can be disconnected from the host computer
and continue running the process (although this would cause the loss of data and
you obviously could not change any settings).
CRN 11/8/95, Rev 7/14/99, Rev 7/21/00, Rev 8/8/01, Rev 8/5/2 Rev 7/30/10
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Procedure for Using Factory Floor™ Software
Important: Log files from Factory Floor are pure ASCII format and are generally large
(>1.5 M) that can be imported to Excel™. Students should bring a flash drive to
copy the files. The procedure for importing files varies with the version of Excel
you are using.
Initializing
1. Turn on computer, the and OPTO Board

2. Open OptoTerm software (listed under OPTO in Programs menu). The PLC in
131 requires that the control software be loaded each time the PLC is turned on.
The PLC in 129 (dedicated for the distillation column) retains programs after
power is turned off.
Loading in 131 (only) Start “Opto Control”, Load the program “C:Program
Files\Opto22\OptoDisp\MIMO0-3-9\MIMO.MMI” Select the “debug” menu
option.
3. elect the controller from controller menu (there is only one controller on each
machine)
4. Open OptoDisplay. Select the display to load (the display is listed in the
experiment
5. Open OptoUtilities/OptoTerm. Click Tools/Start Terminal from the menu.
6. Type "_RUN" in the line and press enter.(use capitals and the underscore,
do not use quotes).
7. When OPTO is running correctly ALL 6 LEDS on top of the PLC are
flashing. And there are NO RED Controls on the control screen.
Running
1. Press "Start/Programs"
2. Select "OptoDisplay Runtime" from the "Factory Floor” program group.
3. Load the appropriate program (if not already loaded)
Saving Data
The control software automatically saves data in ASCII files readable by Excel. The
names of the files are based on the program name and the date. For example, a file
created on September 23, 2010 would have then name RD100923.xxx. are saved on
C:ProgramFiles\OptoDisp\MIMO10-3-9 in 131 and C:Still Data in 129
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Important
UNDER NO CIRCUMSTANCES should students run the other OPTO programs without
the express permission of the instructor. The full suite of Factory Floor software is
included on each machine to allow authorized personnel to modify the software.
FAILURE TO COMPLY WITH THIS RULE CAN RESULT IN DAMAGE TO
THE EQUIPMENT AND SOFTWARE, PERMANENT REMOVAL FROM THE
LAB AND FAILURE FOR THE COURSE.
Rev. 8/11/02 rev 7/30/10
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Statistical Methods in Data Analysis
Ultimately experimental work results in a set of numbers that must be interpreted.

They may in the form of:
a) Multiple measurements of the same thing made in order to be sure we have the
"correct" value
x1, x2, x3,...xn
b) Multiple measurements of two objects that may or not have the same "correct"
value, usually to see if they are identical
x1, x2, x3,...xn, y1, y2, y3,...ym,
c) Multiple measurements involving two variables that influence each other (such as
pressure drop in a pipe, which is a function of flow rate). Such pairs of
measurements are made to see just what the relationship is (proportional to flow,
proportional to the square of the flow, etc.).
(∇P 1, F1), (∇P 2, F2), (∇P 3,, F3),...(∇P n, Fn)
d) Multiple measurements involving three or more variables that are interrelated.

The objective is to determine the functions involved (for example measuring
pressure drop as a function of flow rate in pipes of several diameters D and
lengths L)
(∇P 1, F1), (∇P 2, F2), (∇P 3,, F3),...(∇P n, Fn) at various D’s and L’s
e) The planning of a set of experiments in a situation such as d) above so as to

determine the relationships with the least amount of experimental work
("experimental design")
Frequency Distribution
Our first inclination is to assume that our measurements are exact. If we measure
the temperature of a block of plastic several times we expect to get the same answer. In
fact, we probably will not, within say, 0.1 oF. Even worse, suppose we measure a flow
rate of water from a pipe by catching water in a bucket for a given time using a
stopwatch pressing "START" and "STOP" and then weighing the bucket. We will not
get the exact same flow rate every time because of variations in our response time, spills,
etc.
A good example is given in Owen L. Davies, Statistical Methods in Research and

Production 3rd ed, Ch. 2, Harper, N.Y., 1957, for the measurement of the carbon content
of a powder (see attached pages).
We will find that if we repeat the measurements, say, 178 times we will get a
distribution of values. This distribution can be represented by a HISTOGRAM, which is
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a bar chart whose x-axis is the range of answers divided into equal intervals. The y-axis
is the number of answers falling into a given range.
A histogram can be made easily using quadrille or graph paper or from the table
of data using the function calls in EXCEL, MATHCAD, etc.
If we made a very large number of measurements, the envelope of the histogram

would approach a smooth FREQUENCY CURVE, with the maximum at the true or
average value. If we divide the number of samples in each range by the total number of
samples, we get the probability of finding a sample in that range. With a very large
number of samples, we get a PROBABILITY CURVE.
The curve through the distribution becomes a more accurate representation of the
truth or the UNIVERSE as the number of samples approaches being infinite. There are
several mathematical representations for various curves observed in the world of data.
They are typically expressed in terms of the peak value and the degree to which the curve
spreads out.
If we consider how many of the values are greater or less than a certain value, we
get a CUMULATIVE FREQUENCY DISTRIBUTION. The number of carbon samples
having a content less than any given value is shown in Table 2A-1 and Fig 2A-1 from
Davies. Each value is the sum of the number of samples up to that point.
Arithmetic Mean
The central or peak value of the distribution curve may be close to the ARITHMETIC
MEAN,
N
∑ xi
x= i
N
Occasionally the distribution of data is such that other mean values are useful.
Geometric Mean
The GEOMETRIC MEAN is the Nth root of the product of the observations, which can
be calculated using logarithms:
1
g = ( x1, x2 , x3... x N ) N
N
∑ log( xi )
log( g) = i
N
Harmonic Mean
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It is sometimes better to average the reciprocals of a value (for example the average
density of a mixture), then use the average of the numbers themselves. Thus, the
HARMONIC MEAN of x is
N 1
∑
1 i xi
=
H N
Median
The MEDIAN value is the one for which there is an equal number of observations that
are higher and lower. Thus, the median is the midpoint of the list.
Standard Deviation
A common measure of the spread in the data is the STANDARD DEVIATION

N
∑ ( xi − x )
2
S= i
N −1
As we make more and more measurements, calculated standard deviation approaches that
of the true probability curve and the arithmetic mean approaches the most probable value
 N 
 ∑( x i − x ) 2 
 
σ = lim s = lim  i 
N →∞ N →∞ N −1
 
 
 
µ = lim x
n →∞
These limiting quantities are used in expressing theoretical distributions.
Variance
The VARIANCE V is the square of the standard deviation and is used in more
sophisticated statistical analyses.
Confidence Limits
The ordinate of the probability distribution curve at any point x gives the
probability that the data will fall between x and x+dx. If we consider a shaded area
bounded by the range x-a and x+a, the area represents the probability or fraction of all
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samples that should fall in that range. On a cumulative probability plot, the ordinate at a
given value of x represents the probability, or fraction of samples, that will have a value
of less than x.
Experimental data that fall on a NORMAL DISTRIBUTION curve are

approximated by a mean (peak) value m and standard deviation s. For these
distributions, the probability P that x will lie between µ ± u1σ is given by the following
table taken from Davies.
Method of Least Squares
One frequently encountered problem in engineering is finding an equation to

describe the relationship between two variables x and y. Often, the experimental data
consists of a set of paired data
( x1, y1), ( x2 , y2 ),  ( x n , y n )
We can often describe the relation ship with a linear equation
ycalc = mx + b
where b = the intercept
m = the slope
x = the independent value
ycalc = the dependent value calculated from this equation
In most cases, straight lines through a set of data will not fit all the data exactly; typically
we find something like the graph below
6
0
0 0.5 1 1.5 2 2.5 3
For each data point, we can compute an “error”, ε , or the difference between the
experimentally measured value of y and the value calculated from the theoretical
equation above. Mathematically
ε = ymeasured - ycalc
where ymeasured = the experimentally measured value of the dependent variable
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Statistically, the “best” values for m and b are those that minimize the value ∑ε2 . The
values of m and b that minimize ∑ε2 are found by the Method of Least Squares. The
formulae are
∑ i ( xi yi ) −
( ∑i xi )( ∑i yi )
m= N
( ∑ i xi )
2
2
∑ i xi −( ) N
∑y ∑x
b= i i −m i i
N N
where i = an index that runs from 1 to N
N = the number of data sets
xi and yi are the experimentally measured values for a data point
It is also desirable to measure how good the data fit the straight line that is obtained from
the least squares fit. The “goodness of fit” of the equation is measured by the coefficient
of correlation, r, which is defined by
b ∑ i yi + m( ∑ x y ) −
( ∑ i yi )
2
i i i
2
r = N
( ∑ i yi ) 2
( )2
∑ i yi −
N
where r = the coefficient of correlation
Values of the correlation coefficient range from zero (no relationship between x and y) to
one (perfect fit of the equation). A “good fit” for experimental data in an engineering
system is generally about 0.95.
Rev. 7/17/99, 8/11/02, 7/30/10
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Lab Reports
The Chemical Engineering laboratory courses are designated “Writing Enriched”,
You will submit a total of 25 pages of reports to successfully complete each course.
Your instructor will return your reports for correctiuons.
The Laboratory Report and the Senior Project Report have similar organizations
because both are forms of technical reports. The individual sections of technical reports
are often distributed separately, the abstract being sent to upper management, while other
individual sections are sent to separate branches of the corporate organization. Clarity
and brevity are of utmost importance. Reports will have the following sections in the
order shown. Each section must start on a separate page. Optional items or items required
only on the Final Report are indicated. In addition, your group’s report may contain other
sections (a “Theoretical Analysis” section, for instance).
1. Title Page
this page shows the title of the experiment, the date performed, the date
submitted, authors and team members.
2. Abstract
A concise (normally 200 words or less) statement of the essential contents of
the report for the reader who must get your message in 60 to 90 seconds. The
abstract should include a brief statement of the objective, methods used,
significant results and major conclusions.
3. Introduction
The Introduction is on page 1 of your report. There are several ways of
dividing a document so that there are separate page numbers. The
introduction presents the background of the project and describes how the
project relates to the “big picture”. It should explain fully:
Why the work is being done? (what are the learning objectives)
What has been done previously in the field both at Widener and at other
locations?
What the reader (assume another engineering student) will need to know to
understand your report.
4. Procedure
Describe what was done in sufficient detail that an engineer who was not
associated with the project could duplicate your work.
5. Results
An objective discussion of the principle results and observations from any
experimental work. You are to show that the conclusions are justified. This
is the most important section of the report. Discuss what you have
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accomplished in a positive manner. Do not dwell on minor factors or attempt
to “lay blame” for failures.
6. Conclusions
Conclusions reached in the results are to be restated here in a more general,
less specific manner. In the Interim Report, these are honest answers to the
questions in Section 2. In the Final Report these are the principle things
learned during the project.
7. List of References
8. Appendices (optional)
These can contain sample calculations, computer program listings,
communications, detailed test results
Mechanics and Form

Webster’s Third International Dictionary of English Language (Unabridged) is
the authority for the spelling and usage of words. Expressions cited in this reference as
informal or slang are not acceptable for this report. A copy of this dictionary is available
in the Dean’s Office and in the library. You may also choose to use Webster’s Seventh
New Collegiate Dictionary, which is also suitable.
The Elements of Style, by William Strunk, Jr. and E.B. White, is a good reference
for the rules of usage, principles of composition, and matters of style and punctuation.
The grammar checker in Microsoft Word for Windows is good for helping to proofread
the report. The spelling checker will find many (but not all) typographical errors.
The use of a word processor is required for the text portions of your reports.
Figures and Tables may NOT be hand drawn. You may use Word or any other word
processor of your choice. You may email an electronic version of yor report to your
instructor.
Students having difficulty writing are encouraged to seek help from the Widener
Reading and Study Center.
Format, Pagination and Miscellaneous

All formatting requirements for the reports can be performed using Microsoft Word,
which was used to prepare this manual. See the on line help for Word for details.
1 Paper
White typewriter paper 8 ½ x 11 in without holes. Use one side only.
2 Font
10 point or 12 point (standard typewriter font size) serif fonts (e. g. Times
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New Roman, the font used in this Manual) are required. Suitable fonts should
be used for equations.
3 Margins
One inch on all sides. .
4 Spacing
The text of the Final Report must be double-spaced within paragraphs.
You may find triple spacing convenient for drafts. Most word processors
allow you to easily change line spacing. You may leave an extra space
between paragraphs and between section headings such as in this manual.
5 Pagination
The page number appears at the top center of all pages except the title page,
which does not display a number. Beginning with the Introduction, which is
page 1, the remaining pages, including text, illustrations, graphs, tables and
Appendices should display the page number as an Arabic numeral centered at
the top of a page. Microsoft Word and most good word processors have
automatic page numbering functions.
6 Indentation
Indent paragraphs 5 average character widths or 0.5 inch whichever is most
appropriate.
7 Titles
Titles of books or journals are to be italicized.
8 Endnotes, Footnotes
All paraphrased, summarized or directly quoted material must be identified by
either an endnote or a footnote. Number all such notes consecutively using
Arabic numerals in a single sequence from the beginning to the end of the
report.
9 Tables, Graphs and Charts

These are acceptable and convenient for presenting certain information. They
must be labeled with a number and a title and included on the appropriate lists
alter the Table of Contents. Microsoft Word and several other word
processors have the capability of including tables and graphs in the body of
your report. This approach is both acceptable and convenient because the
word processor will then correctly number the pages. Drawings and
photographs can be included as separate pages not included in the text file or
imbedded in the report. However, a small number of drawings and
photographs may be scanned into the computer, converted to the files and
directly imported into the document. This approach has the disadvantage of
being time consuming and making the document file very large.
10. Appendices
Appendices shall be numbered A, B, C, D etc.
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Drawings for Reports
In preparing your drawings of apparatus with its associated piping and

instrumentation you should tailor the sketch to what you are trying to convey. Neatness
and clarity are more important than a literal picture. A good guide can be found in the
scientific publications such as AICHE Journal or CHEMTECH, where experimental
work is reported. The details of your experimental equipment are important insofar as
they relate to the measurements you are making. A sketch showing pertinent dimensions
and construction is more important than a "pictorial drawing of the outside. Some typical
examples, taken from AIChE Journal, are attached. Similarly, piping can be shown as a
single line, with valves, pumps, etc., shown as the standard symbols given in the attached
sheet.
Occasionally it may be desirable to show a thermometer well or thermocouple

attachment detail as a part of a sketch of the apparatus. More often, an overall flow
diagram can indicate the points and types of measurement by the standard symbols of the
Instrument Society of America. These standard symbols include circles with the
measurement and lines of various types showing where the signals flow. A local
measurement of temperature is a circle with "TI" inside, for example. A controller that
measures temperature, pressure or liquid level and sends a signal to actuate a control
valve is shown in the attached page from Page 171 of Coulson and Richardson, Chemical
Engineering, Vol. 6.
A differential pressure transmitter sending a signal to a computer or controller

can be shown as a circle with "d/P" inside, with a dashed line to indicate the electrical
signal (in our case a 4-20 mA direct current). A sample is shown below.
device d/P
In most cases, free hand drawings of graphs and equipment ARE NOT
ACCEPTABLE in the Final Report. Simple diagrams can be done using various CAD
systems on campus. It is worthwhile to learn how to use one of these. It will take an
afternoon, but is fun. Graphs can be made using a variety of software available on
campus.
JWH 11/17/86 rev. CRN 8/10/00 rev CRN 8/5/02
Experiments
This section contains the experiments you will perform in this lab course. All
students in the group are expected to have read and understood these procedures prior
to the start of the lab. This book is not intended to contain all the theoretical
information you may need to perform an experiment. Before performing any
experiment, you should review the materials in the appropriate course text.
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page 20
It is desirable to bring this manual to class and to the laboratory because the manual
contains specific information about the conduct of the experiments.
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1. Measurement of Viscosity
Objective
To determine the dynamic viscosity of a fluid using a Brookfield viscometer and a

capillary viscometer and to measure the effect of material properties such as temperature
and solution concentration on the viscosity.
Apparatus
1. Brookfield viscometer with small sample adapter, RV 21 spindle

2. Capillary viscometer
3. Stopwatch
4. Assorted glassware, including specific gravity bottle
5. Bausch and Lomb Abbe refractometer
6. Analytical balance (Room 117)
7 Glycerol-water or sucrose-water standard solutions
8. Corn starch, collagen or other material of unknown viscosity
Background
A Newtonian fluid is one where viscosity is independent of velocity gradient (or shear
rate); a plot of stress versus shear rate is linear.
du du
τ=µ =ρ υ
dy dy
where u = the x component of velocity
x and y are Cartesian coordinates
τ = the shear stress (lbf/in2, N/m2)
µ = the viscosity (lbf/ft sec, poise [gm/cm sec])
ν = the kinematic viscosity
A Bingham plastic (most paints or suspensions, for example) does not flow until a certain
yield stress is exceeded; from then on, increases linearly with shear rate:
du
τ = τo + µ p
dy
where τ o = the yield stress
µp = the plastic viscosity
A pseudo-plastic or shear-thinning fluid shows a decrease in viscosity with increasing

shear rate. Dilatant or shear-tinning fluids get stiffer the faster they are stirred. Both of
these fluids are special cases of a power law fluid.
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n −1
du du
τ=m
dy dy
where m = the power law constant
n = the power law exponent
Plots of log(τ ) versus log(du/dy) are straight lines with a slope of n
Plots illustrating these fluids are shown below.
Newtonian Fluid Bingham Plastic Power law

stress
stress
stress
shear rate shear rate shear rate
The apparent viscosity, ma, of a fluid is defined as the ratio between the shear stress, t,
and the velocity gradient, du/dy, for any stress. The kinematic viscosity is m/r, where r is
fluid density.
The viscosity of liquids decreases exponentially with temperature, so that the activation
energy, E, can be calculated from the following equation.
 E 
µ = µo exp  
 RT 
where E = activation energy (Btu/lbmol, kJ/kgmol)

R = ideal gas constant
T = temperature (oR, K)
µo = viscosity constant
Viscosity Measurement
Two common viscometers are the capillary viscometer and the cup and bob
viscometer (such as the Brookfield). In a capillary viscometer, fluid flows by gravity
through a narrow tube, or capillary. In a cup and bob viscometer, fluid is in a stationary
cup. A cylindrical bob is lowered into the cup and rotated. The torque and rotational
speed are the noted. This type of viscometer is often called Couette or Couette-Hatschek
viscometers
Fig. 1 Schematic of a cup and bob viscometer
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Rotating bob
Gap filled
with fluid
Stationary Cup
Capillary Viscometers (Couette viscometers)
Flow in a capillary viscometer is usually laminar. Direct calculation of the flow

can be performed using the equation for laminar flow in a pipe (6).
π ρghR 4 V
Q= = (1)
8µL t
where g = the local gravitational acceleration

h = the head of liquid
t = the time for a volume, V, of liquid to flow through the capillary
L = the length of the capillary
Q = the volume rate of flow
V = a measured volume of liquid that flows through the capillary
ρ = the fluid density
µ = the viscosity
However, such calculation is often inaccurate because of imperfections in the

diameter, entrance effects, etc. More often, the viscosity of an unknown fluid is found
by measuring the time for a know volume of fluid to flow through a viscometer. This
time is compared to the time for the same volume of a known standard to flow through
the same viscometer. From equation 1, it is easy to show that
ρ t
µ = µs (2)
ρs t s
where µ, ρ, and t are the viscosity, density and time for the unknown and µs, ρs
and ts are the viscosity, density and time for the standard material.
This equation is often written in terms of the kinematic viscosity
t
ν = νs (3)
ts
where υ and υs are the kinematic viscosity of the unknown and standard
respectively.
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Cup and bob Viscometers
The cup and bob viscometer, illustrated above, allows direct measurement of the
viscosity of a fluid. Standards can still be used for accurate calibration. Furthermore, at
higher Reynolds numbers the flow is unsteady (called Taylor instabilities). Nonetheless,
at low Reynolds numbers flow closely follows the theoretical model. Furthermore,
because stress is nearly uniform across the gap between the cup and bob, the plot of shear
stress, vs. shear rate plot can be made. This last feature is most useful when measuring
NonNewtonian fluids.
For a cup and bob viscometer, the flow equations can be solved to yield (6)
 κ2 
T = 4πLΩR 2   (3)
1 − κ
2

where L = the length of the bob
R = the radius of the cup
κ = the ratio of the bob radius to the cup radius
Ω= the rotational speed (in radians/sec)
The shear stress and strain rate can also be calculated. They are
− 2µΩ  κ2 
τ=   (4)
κ2  1 − κ 2 
dv θ 2Ω
θr = =− (5)
dr r κ2 −1
where τ = the shear stress
θ = the shear rate (in sec-1)
General Procedure
1. Measure density and temperature of standard solution and undiluted Karo syrup.
Look up concentration in table (see bulletin board)
2. a. Read shear stress, viscosity of standard and undiluted Karo syrup versus rpm
using the Brookfield viscometer, at room temperature.
b. Compare measured value of standard's viscosity with literature value.
3. Measure the viscosity of the Karo syrup in the same manner as a function of
temperature over as wide a range as is practical (from about 25C to 50C), using
the Brookfield viscometer.
4. Measure the viscosity of oatmeal, mustard or whatever material your instructor

provides at 30C.
5. Dilute the Karo solution with distilled water by about 25%; be sure to blend the
mixture thoroughly. Measure the specific gravity and the viscosity with the
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Brookfield unit at room temperature. Repeat until the viscosity has fallen to
about 200-400 cp. This is the "unknown" solution for the capillary viscometer.
Measure its specific gravity and estimate its concentration.
6. a. Measure time of flow through the capillary viscometer for the standard and the
unknown solution.
b. Calculate the viscosity of the unknown solution by comparing flow time with
that of the standard. Compare the result with that from the Brookfield.
Treatment of Results
1. Plot shear stress versus shear rate for the standard solution, the sucrose solutions
and any other material examined in the Brookfield.
2. Plot viscosity vs. temperature and viscosity vs. concentration. Discuss the effects
of temperature and concentration on viscosity, comparing your results to any
correlations in the literature. Use the appropriate type of plot. For instance,
when plotting viscosity vs. temperature use the plot that would give a straight line
if you were trying to find the activation energy.
3. Estimate the diameter of the capillary, neglecting end effects.
References:
1. Brookfield Instruction Manual.

2. Crosby, O. J., Experiments in Transport Phenomena, pp. 1-5, John Wiley, New
York, 1961.
8. Reid, R. C., J. M. Prausnitz, and B. O. Poling, The Properties of Liquids and
Gases, pp. 434-440, 4th ed., McGraw-Hill, N.Y., 1987.
9. Tanner, R.I., Engineering Rheology, Clarendon Press, Oxford, 1985
10. Bird, R. Byron, W. E. Stewart, and E. N. Lightfoot, Transport Phenomena, pp.
94-96, Wiley, N.Y., 1960
JWH rev. 1/10/94
CRNrev. 1/6/96 rev. 7/17/99
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2. Friction Loss in Pipes and Fittings
Objectives
To demonstrate an understanding of procedures for instrument calibration and the
experimental basis for turbulent flow correlation. To demonstrate an understanding of
the use of equivalent length by measuring its value.
Apparatus
1. Scott Model 9009 Fluid Circuit System, using circulating water.
2. Stopwatch, pail, and platform scale
Background
The mechanical energy balance between two points in a system through which fluid is
flowing is given by the modified Bernoulli equation (equation 1)
gz1 v12 P1 gz2 v22 P2
+ + = + + + lw12 (1)
g c 2 gc ρ gc 2 gc ρ
where 1 and 2 are the two points
g = the local acceleration due to gravity (32.2 ft/sec2, 9.8 m/sec2)
gc = 32.2 lbf sec2/(lbm ft) = 1 N sec2/(kg m)
lw12 = the energy dissipated by viscous flow (ft lbf, kJ)
v = velocity (ft/sec, m/sec)
P = pressure (lbf/ft2, Pa)
z = elevation relative to a datum (ft, m)
If the flow is incompressible (if the material's density does not change) in a level, straight
pipe of uniform diameter, equation 1 reduces to:
lw12 P −P
= hf = 1 2 (2)
g ρg
where hf = the “head loss” or pressure drop (ft, m)
The head may be thought of as the height of liquid that would be supported in a
manometer attached to the pipe. Thus, a manometer connected to two points on a
horizontal pipe measures hf directly.
A large number of experiments using many pipes and fluids have resulted in a
correlation of the data using the friction factor f. The Fanning friction factor is defined
by equation 3.
2 fLv2
hf = (3)
gc D
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where D = the inside pipe diameter (ft, m)
f = the Fanning friction factor (dimensionless)
L = the length of pipe (ft, m)
The friction factor is a function of the Reynolds number and the roughness of the
pipe, as shown in figure 1 below.
Fig. 1 Moody Chart
from .J. R. Welty, C. E. Wicks, and R. E. Wilson, Fundamentals of Momentum, Heat,

and Mass Transfer, 3rd edition, Ch. 14, John Wiley, New York, 1984
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Note that the roughness of the pipe is expressed as the dimensionless ratio ε/D,
where ε is the roughness of the material and D is the pipe inside diameter.
Losses in pipefittings can be correlates equivalent lengths, L/D, or a loss factor K

that replaces the group (4fL/D). Valve capacity (essentially the inverse of resistance to
flow) can be expressed as a coefficient Cv as in the attached sheets.
General Procedure
1. The team should familiarize themselves with the locations of the various valves
on the apparatus before attempting to obtain data.
2. Calibrate the venturi and orifice flow meters by measuring the time to fill the
bucket with a stopwatch. Weigh the bucket to determine the mass of water.
Repeat this procedure for at least 5 different flows.
3. Determine the pressure drop across a portion of the piping system as a function of
flow rate over as wide a range of flow rates as possible.
Treatment of Data
1. For straight tubing, calculate the friction factors at the various flows and compare
with values obtained from the literature.
2. For the valves and fittings, calculate the equivalent length and loss coefficient (K)
and compare with values from your textbook.
References
1. C. O. Bennett and J. E. Myers, Momentum, Heat, and Mass Transfer, 3rd ed., pp.
197-209, McGraw--Hill, New York, 1982.
2. F. M. White, Fluid Mechanics, pp. 302-316, McGraw-Hill, New York, 1986.

(Note the use of Darcy friction factor rather then Fanning friction factor.)
3. R. H. Perry, D. W. Green, and J.O Maloney eds., Chemical Engineer's

Handbook, 6th ed., Sec. 5, pp. 20-25, 37-39, McGraw-Hill, New York, 1984.
4. J. R. Welty, C. E. Wicks, and R. E. Wilson, Fundamentals of Momentum, Heat,

KMM/JWH 5/23/83
rev. 1/20/94
CRN rev. 1/9/96 rev 8/11/02
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3. Transient Response of Two Interacting Tanks
Objective
To demonstrate knowledge of how to empirically determine properties for a process by

setting up a test for a level control system of interacting tanks.
Apparatus
1. Two surge tanks equipped with level transmitters
2. 30-gallon sump tank and recirculating pump
3. Rotameter for measuring flow to first tank and sensors for measuring flow into
the
. first tank and out of the second
4. Dell computer, OPTO LCSX hardware and Factory Floor software
The resistance to flow between the two surge tanks can be adjusted by means of a valve.
The instructor sets this valve at the star of the experiment. DO NOT ADJUST THIS
VALVE. The values determined in this experiment will be used in later experiments.
Background
The configuration of the two-tank system is shown in Figure 1:

The differential equation that describes flow in a tank is:
dM
=m
 in − m
 out (1)
dt
where M = the mass of water in the tank
m
 in = the mass flow rate into the tank
m
 out = the mass flow rate out of the tank
The mass in a cylindrical tank is related the volume through the equation
M = ρAh (2)
where A = the cross section of the tank
h = the height of liquid in the tank
ρ = the density of water
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Figure 1
Sketch of Two Interacting Tank Apparatus
Surge
Tank 1
Surge
Tank 2
Automatic valve 1
Manual valve
Automatic valve 2
In free drainage, such as the flow out of the first tanks, the flow is a function of the
difference between the height of liquid in the tank and the height of the level of the
discharge:
 12 = f ( h tan k − h out )
m (2)
For turbulent flow the flow rate is approximately:

 12 = ρk t12 h 1 − h 2
m (3)
where kt12 = a constant based on the conditions of turbulent flow
On the other hand, laminar flow yields equation 7

 12 = ρk lam12 ( h 1 − h 2 )
m (4)
where klam12 = a constant based on the conditions of laminar flow
A similar set of equations may be written for the discharge from surge tank 2
 2 = ρk t 2 h 2 − h d
m (5)
 2 = ρk 1am 2 ( h 2 − h d )
m (6)
where kt2 = a constant for the discharge geometry and turbulent flow conditions
klam2 = a constant for the discharge geometry and laminar flow conditions
m 2 = the mass rate of discharge from surge tank 2 (lb/sec, kg/sec)
zd = the elevation of the discharge from surge tank 2 (ft, m)
A material balance around each tank yields.
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dM1
=m f −m 12
dt
(7)
dM2
=m 12 − m
2
dt
where M1 and M2 are the masses of water in surge tank 1 and surge tank 2 respectively
m f = the flow into surge tank 1
To determine the flow constants for the tanks, we will consider the steady state case. For
tank one in laminar flow.
ρF = k lam12 ( h 1 − h 2 ) (8)
where F = the volumetric flow rate
and for turbulent flow
ρF = k t12 h 1 − h 2 (9)
Similar steady state equations are valid for tank 2. You should write them yourself.
Determine whether the flow is laminar or turbulent
The formula to calculate laminar and turbulent flow constants can be easily written.
However, we cannot determine whether the flow is laminar or turbulent from
measurements at a single flow rate. Nor can we determine the type of flow without
taking apart the valve and examining its internal parts at their current setting (something
we would rather not do while the process is running). The flow constants, however, are
independent of the flow rate or level. Therefore, it is possible to determine which flow
description (laminar or turbulent) best describes the flow by repeating the measurements
of them at several different steady state conditions and noting which flow constant, klam12
or kt12 changes the least over a wide range of flows
General Procedure
1. Establish reasonable and steady levels in the two surge tanks by adjusting the
input flow.
2. Repeat at least 5 times at different flow rates. Do not overflow the tanks.
3. When the flow is at steady state, change the input flow suddenly to a new value,
and follow the change in tank levels until a new steady state is reached. You will
compare the response of the system to a flow change to a theoretical model you
develop using the flow and k value determined from the data in parts 1 and 2.
1. Determine the relationships between the head differential and flow in the
interconnecting piping (k12 and k2). Use steady state conditions.
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2. Determine which flow, laminar or turbulent best describes the flow out of tank
one and tank two by noting which flow constant is most constant over the range
of flows.
3. Use your chosen flow constants to model the unsteady state data you obtained
when you performed step 3 in the General Procedure. The software in the
Appendix below will be helpful.
CRN Rev. 1/8/96, 8/30/99, 8/22/00, 8/5/02
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4. Level Control of Tanks
Objective
To demonstrate knowledge of controller tuning procedures by tuning the PID controllers

in the interacting tanks apparatus.
Apparatus
1. Two (2) 0.01 m3 surge tanks equipped with level transmitters

3. Rotameter for measuring flow to the first tank
4. Dell computer, OPTO LCSX hardware and Factory Floor software.
The resistance to flow between the two surge tanks can be adjusted by means of a valve.
A sketch of the setup is shown below
Figure 1
Sketch of Two Interacting Tank Apparatus
Surge
Tank 1
Surge
Tank 2
Automatic valve 1
Manual valve
Automatic valve 2
Background
The three common modes of control using conventional PID controllers are
proportional (P), proportional integral (PI) and proportional, integral derivative (PID)
based upon the algorithm used to change the controlled variable. The algorithm uses
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input to the controller to calculate the controller output (a signal to the valve). The
“input” to the controller is a signal representing some variable, such as tank height and a
“set point” or desired height. The difference between these two is a deviation from the
set point.
ε = Imeasured - Iset
where Imeasured = the measured value of the input signal
Iset = the set value of the input signal
ε = the deviation from the set point
For instance if the set point is 20 inches of height in tank and the actual elevation
is 22 inches, then the deviation is +2 inches.
1. Proportional Control
For proportional control, the output from the controller is just proportional to the
deviation
O = KPε
where KP = a constant (often called the gain) to be determine for the process
O = the output from the controller.
The output from the controller is a signal that does something to the process, for
instance opening or closing a valve. Because the controlled thing operates over a finite
range, the output is often expressed as a percentage of full scale. For instance, if the
output controls a valve, it can range from 0 (fully closed) to 100 (fully open).
2. Proportional Integral (PI) Control

A more sophisticated type of control is called proportional integral control, which
can be described by the following equation
O = K P ε + K I ∫ε( t )dt
where KI = a constant for the integral portion of the controller to be determined for the
process
3. Proportional Integral Derivative (PID) Control

The most sophisticated type of controller other than specialized “smart”
algorithms requiring digital computers (such as fuzzy controllers, and artificial
intelligence) is a PID control
dε
O = K Pε + KI ∫ ε( t )dt + K D
dt
where KD = a constant for the derivative portion of the controller to be determined for the
process
Assume that a proportional controller operates valve 2, the drain valve. At an

initial steady state, the control valve is set to a position that gives the desired level in the
tank and the controller is activated. If, because of a change in the inlet flow, the level
exceeds the set point, the drain valve will open. The height of liquid in tank 2 will reach
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a new level. Depending upon the value of KP, the new level may be close to the set point
but will not be exactly the set point. The difference between this new steady state value
and the set point is called offset.
If the value of KP (the gain) is too high, the system may become unstable and may
cycle around the set point. Such a situation is called “overcorrecting” or “overshooting”.
The valve position at the new steady state can be shifted to the position required
to restore the level to the set point by adding integral control (making KI non zero).
Systems with a lot of “inertia”, which tend to overshoot the set point when
approaching it, can be controlled better by adding derivative action (making KD
nonzero). This causes the valve position in the example to be changed according to the
rate at which the height approaches the set point.
Another type of simple controller is on/off, or bang/bang control. Engineers use

on/off control when equipment can only function easily in an on/off manner. An
example is a house thermostat that controls a heating furnace that can only function in a
“fully on” or “fully off” manner.
Most process control texts give detailed descriptions of the process for
determining the control constants.
General Procedure
1. Your Instructor will designate the control configuration to be used. Typically,

control schemes are outlined below:
Control the level of surge tank 2 using the output valve
Control the level into surge tank 1 using the input valve
The process disturbances are either a change in the flow rate (a “wild” or external
variable) or a change in set point.
You will need to measure the response of the system to changes in the
manipulated variable (the valve position). A list of methods is provided in the
Process Control section of the Virtual Lab. Your instructor may suggest a tuning
method. You should examine “First Order Plus Deadtime” and “Autotuning” on
the instructions page when preparing for this lab.
2. Tune the controllers using each of the control techniques found on the Online
Widener Laboratories. Determine the P, PI and PID settings.
3. For each of the settings obtained in 2, line set the controller on “Automatic” with
the system running steadily. Then, change the input flow up and down by at least
10% and wait for new steady states. Repeat by changing the set points at several
fixed flows.
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4. Determine the %overshoot and rise time for each setting.
5. With the controller on automatic, change the flow/position of the other controller
by at least 10% and determine the response.
Report
1. If you developed a “process model” for tuning the controller, include it and the
data you used in developing it in your report. Would you need more than one
process model? If so why, if not why not.
1. Plot the responses of the systems to changes in setpoint and changes in flow/valve
position. Is there some flow/valve position of the other valve (the “wild” or
uncontrolled variable) that prevents the PI and PID controllers from maintaining
the set point? (that is, did you find an “operating window” for the process).
2. What was the proportional offset for the P controller?
2. Plot controller output as a function of deviation from the set point.
3. Discuss the effect tuning method. Which method gave the most aggressive tuning
settings?
JWH 9/28/93 rev. 1/11/94, CRN rev. 1/10/96, CRN rev 8/8/1 rev 8/11/2 rev 7/30/2010
36
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5. Frequency Response of a Control System

Objective
To demonstrate knowledge of frequency response by experimentally measuring a Bode

plot.
Apparatus
1. Two (2) 0.01 m3 surge tanks equipped with level transmitters

3. Rotameter for measuring flow to the first tank
4. Dell computer, OPTO LCSX hardware and Factory Floor software.
General Procedure
1. Your Instructor will designate the control configuration to be used. Typically,

control schemes are outlined below:
Control the level of surge tank 2 using the output valve
Control the level of surge tank 1 using the input valve
The process disturbances are either a change in the flow rate or a change in set
point.
2. Your instructor will specify whether you are to perform the experiment in open
loop (controllers on manual) or closed loop (controllers on automatic) mode. For
open loop measurements, set the PID output to some reasonable value that does
not drain either tank completely or cause an overflow.
Connect the sine wave generator to be the forcing function for the valve not
controlled by a PID controller.
3. Set the “offset” level on the sine wave generator to some intermediate value that
keeps the tank levels and flows in approximately the middle of their ranges. All
other values on the sine wave generator should be 0
4. When the system is at steady state, set the period to a reasonable value and
increase the amplitude. The sine wave generator will vary the valve
position. Allow the system to reach a steady oscillation. Measure the
phase shift and amplitude response for the controlled liquid height to sine
wave signal.
5. Repeat step 5 for at least 5 different periods.
Report:
1. From your data construct Bode plots for your system. Is there a frequency that
can cause instability for this system? Would you expect such a frequency?
CRN 8/8/1, 8/5/2
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8. Heat Conduction in Solids
Objective
To demonstrate an understanding of heat conduction in solids and free convection by

correctly performing calculations for four different experiments.
Apparatus
1. Scott Model 9051 Thermal Conduction System

2. Factory Floor ™ and OPTO 22 programmable logic controller (PLC)
See "Procedure for Using Paragon 500" in this manual for general
instruction on configuring the computer.
3. Digital thermocouple indicator
4. Thermometer
Background:
The Scott Model 9051 Thermal Conductor system has several units, each of
which is described below.
1. Tube Furnace Unit

A tube furnace is arranged to heat a special high temperature 18-8 stabilized
stainless steel bar. On each end of the bar are two segmental metal bars forming
extensions of the stainless bar and arranged so that heat will flow through these
components. Each of the segments is of different material.
One end of one conductor assembly terminates in a heat sink that is water-cooled.
Entrance and exit temperatures of the cooling water are measured. The assembly is
encased in a double cylindrical insulating jacket. The other assembly is a “fin”.
All segmental metal bars are provided with thermocouples spaced longitudinally
so that temperatures may be measured along the path of heat flow.
2. Variable-Area and Constant-Area Conductor Units

A variable-area conductor is enclosed in an insulated cylinder, so arranged that
the smaller and lower end of the conductor may be heated by a hot plate. The upper end
of the conductor terminates in a heat sink that is water-cooled. Thermocouples indicate
the temperature at the center of the conductor. They are spaced vertically along the
length of the conductor.
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A second insulated cylinder similar in design to the variable-area unit forms a
housing for a constant-area conductor. This unit is heated at one end and cooled at the
other. It is instrumented in the same way as the variable-area unit.
3. Unit Selector and Thermocouple Selector Switches

A selector switch is provided for selecting between conductor experiments. A
thermocouple selector switch enables individual thermocouples to be wired to the
indicating instrument.
Background
In the Scott apparatus, nearly all the heat is flowing longitudinally through a rod.
Heat loss in the radial direction can be assumed small enough that there is a negligible
radial temperature gradient in the metal. Thus, the one dimensional heat conductance
equation can be assumed in the L direction.
dT
q = − kA (1)
dl
where A = the cross section of the conductor (ft2, m2)
 Btu W 
k = thermal conductivity  , 
 hr ft o R mK 
 
l = longitudinal direction (ft, m)
This equation assumes that there is no radial heat loss. Therefore, q is assumed to be
constant over the entire length of the rod and
q L dl T2
∫ = ∫T dT (2)
k 0 A 1
where L = the length of the rod (ft, m)

T1 and T2 are the temperatures at the ends of the rod
In the case of the tapered rod, A is a function of l. If the change in the cross is
gradual, heat flow can still be considered one dimensional, and temperature can be
assumed a function of l only.
If there is appreciable, but relatively small heat loss to the surroundings in the
radial direction, q is no longer constant. Its rate of change becomes
d 2T
kA = q rAo (3)
dl2
where Ao = the outside area of the rod per unit length of rod (ft2/ft, m2/m)
 Btu W
qr = the radial heat loss per unit length of rod  , 
 hr ft m
 
The outside heat loss of the exposed fin is made up of convection and radiation losses:
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( ) (
q r = hcA o T − Tsurroundin g + εA oσ T4 − Tsurroundin
4
) (
g = hc +R T − Tsurroundin g ) (4)
 Btu W 
where hc = free convection coefficient  
 hr ft 2 o R m2 K  ,
,
 
1
 T − Tsurroundin g
4
 Btu 
hc = 0.27    
 D   hr ft 2 o R 
D = the outside diameter (ft, in)
hc+R = the “effective” heat transfer coefficient taking into account both convection
and radiation
T = the temperature at any point along the rod (assumed to be a function of l
only)
Tsurrounding = the surrounding temperature
ε = emissivity
Btu
σ = Stefan-Boltzman constant = 0.1713 × 10−8 2 o 4
ft hr R
If hc+R or qr is approximately constant, equation 3 can be integrated to give the

temperature profile. If not a stepwise integration of equations 3 and 4 is required. It
should be noted that equation 1 gives the longitudinal heat flow at any point along the
length of the rod.
General Procedure
Each experiment should be carried out at two levels of furnace temperature.

Heater should be turned on an hour or two before the laboratory period. Data is taken
when temperatures indicate steady state.
Make a tabulation of the thermocouple temperatures and the inlet and outlet water
temperatures and the cooling water flow rate, as determined with the beaker and
stopwatch. The heat carried away by the cooling water is
q = wC P ( Tout − Tin )
where CP = the heat capacity of water (Btu/lboR, J/kgK)

Tin = the inlet cooling water temperature
Tout = the outlet cooling water temperature
w = the mass rate of water flow (lb/sec, kg/sec)
Results:
1. Conduction through rods in series:

1. Plot the temperature of the conductor versus distance from the furnace
end.
Btu
2. Assume a value of k = 220 for copper
hr ft o R
40
page 41
3. Compute the heat transferred away through cooling water at the water-
cooled end of the unit
4. Compute the heat transferred through the copper component of the series
conductor and compare with the value obtained from step 3.
5. Compute the value of k for the other material in the conductor based on
the ratios of dT/dl in the two different sections.
2. Conduction in the rods with variable and constant cross section:

Compare the temperature profile in the two vertical rods to a calculated
distribution based on the top and bottom temperatures.
3. Conduction in the exposed rod:

1. Assuming values of conductivity from the literature, calculate and plot the
longitudinal heat flow and heat loss qr as a function of l, position down the
rod.
2. Calculate hc+R as a function of Tsurrounding - T and compare with the equation
for hc.
References
1. C. O. Bennett and J. E. Myers, Momentum, Heat, and Mass Transfer,

3rd Edition, Ch. 17, pp. 442-443, 465-471, McGraw-Hill, New York, 1982.

JWH/KMM 7/2/85
rev. 7/28/93
CRN rev. 1/10/95
CRN rev. 7/14/99, 8/5/2
41
page 42
9.Unsteady State Heat Transfer
Objective
To demonstrate knowledge of unsteady state heat transfer calculations by performing

those calculations using graphical techniques.
Apparatus
1. Several solids of cylindrical, spherical, or cubical shape; the solids have 1/16 inch
holes drilled to receive thermocouples.
2. Thermocouples
3. Thermocouple readout Factory Floor ™ and OPTO LCSX programmable logic
controller (PLC)
Background
The temperature distribution inside a solid in which there is no internal heat

generation can be found from the Fourier field equation:
∂T k 2
= ∇ T
∂t CPρ
where CP = heat capacity (Btu/lboR, W/kgK)
k = thermal conductivity (Btu/(hr ft oR), W/(m K))
t = time (sec)
ρ = density (lb/ft3, kg/m3)
The group k/CPρ is the thermal diffusivity. This equation has been solved for simple
geometrical systems with appropriate boundary conditions. In one dimension the
Fourier equation is
∂T k ∂2 T
=
∂t CPρ ∂x2
where x = a spatial coordinate
The heat flux normal to a given cross section is given by
∂T
q x = − kA
∂x
where A = the area of the cross section (ft2, m2)
qx = the heat flux (Btu/hr, W)
42
page 43
Analogous forms exist in cylindrical and spherical coordinate systems.
If a film surrounds the external surface with a temperature drop across it, the
surface temperature, which determines the boundary condition, is given by
qx dT
= −k = h( T∞ − T0 )
A surface dx surface
where h = convective (plus radiation) heat transfer coefficient from surface to

surroundings
T∞ = (constant) surrounding temperature
T0 = surface temperature
The solution to this equation has been obtained analytically and is found in many
textbooks in a graphical form often referred to as the Gurney-Lurie charts. These charts
use the following terms to describe the temperature profile.
T∞ − T
Y=
T∞ − To
αt
X= 2
x1
x
n=
x1
h
m=
kx1
where h = the heat transfer coefficient of the liquid
k = the thermal conductivity of the solid
n = relative position (a value of the charts)
m = relative thermal resistance (a value on the charts)
t = time
T = local temperature
To = the initial temperature
T∞ = the final temperature
X = relative time
x = length
x1 = a key dimension, such as radius, the exact definition is specified on each
chart
Y = unaccomplished temperature change
k
α = thermal diffusivity =
ρCP
CP = heat capacity
ρ = density
43
page 44
The ratio m represents the relative resistance of the outside film l/h to the
resistance of the path of longest distance for heat flow x1/k. The differential equations
have been solved for various geometric shapes and values of m, n, X and Y. Solutions
are presented in the references.
Where heat flow is in more than one direction, the solutions in terms of
dimensionless temperature approach for each dimension, can be combined by Newman's
rule of multiplication to give the resultant solution.
Y3D = YxYyYz
where Yx, Yy, and Yz are evaluated for the x, y and z directions at time t
Y3D = the numerical solution of the three dimensional problem
For example, a rectangular solid of dimensions 4 inches by 2 inches by 1 inch is made up
of the intersection of three semi-infinite solids perpendicular to each other. Each semi
infinite sold is of half thickness 2, 1, and 0.5 respectively.
Thus, a measured Y for a given cube could be converted to the one-dimensional

equivalent for the same m, n by taking its cube root. This value can be compared to the
one-dimensional graphical or analytical solution.
General Procedure
1. Prepare a sketch of the wiring of the thermocouple system showing the locations
of the thermocouples. Data will be recorded using Factory Floor™.
2. Measure the dimensions of the objects supplied and make a sketch, showing the
location and depth of thermocouple openings.
3. Measure the density of the materials.
4. Place the samples in steam bath and turn on the steam. Follow the center
temperature until it equals the oven temperature.
5. Shut off the steam and turn on the cooling water. Measure the temperatures at the
various locations in the solid as a function of time until it approaches the water
temperature.
Treatment of Results:
1. If the properties of the material are known from the literature, estimate m and
compare the cooling curves with those calculated from a Gurney-Lurie chart (or
analytical equation, if desired).
44
page 45
2. If the measured surface temperature differs greatly from the surroundings
temperature, estimate the value of m from the data and if m is large enough,
estimate the outside film heat transfer coefficient h.
References

3rd Edition, Ch. 19, McGraw-Hill, New York, 1982.

JWH/KMM
rev. 5/15/86
CRN rev. 1/6/96, 8/22/00, 8/4/2
45
page 46
10. Film and Dropwise Condensation
Objective
To demonstrate knowledge of heat transfer calculations by measuring the heat transfer

coefficient for steam condensing on the outside of a horizontal tube in film and dropwise
condensation modes.
Apparatus
1. Scott Model 9055 Film and Drop Condensation System

2. Boiler
3. Potentiometer or digital thermocouple readout
4. Weighing vessel and scales
The Condensation Unit is in a long box with solid walls on three sides and the
ends. Sealed glass doors in heavy frames enclose the front side.
Copper cooling tubes extend the length of the box, emerging at both ends. The
cooled surface is 34 in. long, 5/8 in. in diameter.
The apparatus has two cooling tubes are provided, one with a matte surface and
the other with a highly polished surface. A water supply line is fitted at one end of each
tube. A flowmeter measures the water flow rate in the cooling tube. A drain is attached
to the opposite end of the cooling tube. A line supplies steam to the box, and a drain line
is provided to drain condensate from the box. A pressure-limiting device and manometer
are located on top of the box. A highly polished metal reflecting plate inside and behind
the cooling tube also helps in the observation.
Thermocouples are arranged to measure the cooling water temperatures near the
inlet and the outlet of the cooling tube, and other thermocouples are placed to measure
the outside-surface wall temperature of the cooling tube.
Background
The classic analysis of film-type condensation by Nusselt assumes that the latent
heat of condensation passes by conduction through a film of liquid to the tube wall. The
liquid film may be flowing in laminar or turbulent flow, depending on the Reynolds
number. Equations correlating existing data are given in the references.
The overall heat transfer coefficient for a tube is given by the equation
1 1 ∆r 1
= + + (1)
UA o h o A 0 k w A lm h i A i
46
page 47
where Ai = the inside tube wall surface area (m2)
Alm - the log mean of the inside and outside wall area (m2)
Ao = the outside tube wall surface area (m2)
hi = the inside heat transfer coefficient (J/m2 sec K)
ho = the outside heat transfer coefficient (J/m2 sec K)
U = the overall heat transfer coefficient (J/m2 sec K)
∆r = the tube wall thickness (m)
If the flow is turbulent, the inside heat transfer coefficient can be determined from the
Dittus Boelter equation (ref. 3, p. 366)
Nu = 0.023 Re 0.8 Pr 0.4 (2)
where Nu = the Nusselt number (hiD/k)
Re = the Reynolds number (ρVD/µ)
Pr = the Prandtl number (µCp/k)
The outside heat transfer coefficient depends upon the nature of the condensation and is
only slightly dependent on flows. On most surfaces, water condenses in sheets,
completely wetting the tube wall. In the case of horizontal tubes, the outside heat
transfer coefficient can be obtained from the equation of Nusselt (ref. 3, p. 395)
[
 ρ L g( ρ L − ρ v ) k L 3 h fg − 83 C pL ( Tsat − Tw )
h o = 0.725
]  0.25
 (3)
 µ L D( Tsat − Tw ) 
where CpL = the heat capacity of the liquid
D = outside diameter
hfg = heat of vaporization of the liquid
kL = thermal conductivity of the liquid
Tsat = the saturation temperature of the condensing vapor
Tw = the wall temperature
µL = the viscosity of the liquid
ρL = the liquid density
ρv = the vapor density
Dropwise condensation occurs when the metal surface is not wetted by the
condensate. It is difficult to obtain consistently, but when it does occur, the average heat
transfer coefficient is much higher than with film condensation.
 0.8 over the normal range of flows. Equation 2 can,

From equation 2, we note hi ∝ m
therefore, be rewritten as:
1 1
= R steam + R wall + R fouling + (4)
Uo cm 0.8

where c = a constant for a particular set of conditions

Rfouling = the thermal resistance due to fouling (assumed negligible)
Rsteam = the thermal resistance on the steam side of the exchanger
47
page 48
1
R steam =
h0A0
Rwall = the thermal resistance due to the tube wall
∆r
R wall =
k w A lm
Wilson, in 1915, recognized that equation 4 provides a simple means for determining the
steam and wall resistance. The Wilson plot is a graph of 1 U versus 1 0.8 has a
o m
R
slope of 1/c and an intercept equal to steam + R wall + R fouling . The wall thermal resistance
(Rwall) can be calculated easily. If both inside and outside surfaces are clean, the fouling
resistances are small and the intercept is equal to (Rsteam + Rwall).
In any heat exchange measurement it is desirable to estimate the heat transferred using
measurements of both hot and cold streams. The amount of heat flowing from one
stream to another is based on these two measurements. Normally, heat transfer
coefficients are calculated assuming that the more reliable value of heat flow is correct.
The average of the two measurements is used if they are close.
In this experiment there two experimental values of the rate of heat transferred to the
water (q):
1. From the circulating flow through the heat exchanger and its temperature rise
2. From the rate of steam condensation and the latent heat released
General Procedure
It is important to bleed air from the condensing chamber and leave the vent OPEN.
1. Turn off cooling water to the tubes and measure condensate rate as a check on
chamber heat loss to the room when no water is running through the tubes. Do
not forget this step.
2. The experiment is conducted with cooling water passing through each tube
separately. Saturated steam is admitted into the box and cooling water is started
through the flow meter and cooling tube. After a stabilized condition of flow has
been established, the character of the condensation formation is observed on the
outside of the cooling tube. All temperature readings are taken and the water rate
is recorded. Record the amount of condensate. Several runs are made at different
cooling water flow rates. You should try to make at least three runs and you must
exceed the range of the rotameter to get a wide range of flows.
3. Perform step one with both the polished and the matte tubes.
Treatment of Data
48
page 49
1. Calculate the chamber heat loss.
2. Calculate a heat balance for each run, comparing the heat removed by the cooling
water with that lost by the condensing steam, as determined by the mass of
condensate.
3. Calculate film coefficients and compare with literature correlation.
4. Why is it important to eliminate air? Why do you feel air is or is not present in
the chamber during your experiment.
References

3rd Edition, pp. 414-424, McGraw-Hill, New York, 1982.
2. W. L. McCabe, J. C. Smith, and P. Harriott, Unit Operations of Chemical

Engineering, 4th Edition, pp. 333-343, McGraw-Hill, New York, 1985.

JWH/KMM 8/03/83
rev. 7/28/93
CRN rev. 1/6/96, 3/30/00, 8/22/00, 8/6/2
49
page 50
12. Tray Column Efficiency, Technovate Column
Objective
To demonstrate an understanding of fundamentals of distillation by measuring the overall

plate efficiencies in a laboratory tray column.
Apparatus
1. Technovate Model 9079 distillation column, with electrically heated reboiler, 7

sieve trays, condenser, product accumulator/reflux drum, pumps for supplying
reflux or feed, and approximately 13 L reboiler.
2. Dell computer, Factory Floor software, and OPTO 22 programmable logic

controller (PLC) for monitoring temperatures and controlling the Technovate
column.
3. Specific gravity bottles, refractometer, or other appropriate analytical instrument

such as gas chromatograph.
Background
Tray efficiency measurements for distilling systems are most easily made at total
reflux. For simple systems where the relative volatility is constant, the spread between
the top and bottom compositions is given by the Fenske-Underwood equation:
xAD N xAN
= α AB
xBD x BN
where N = the number of the theoretical stages in the system
xAD, xBD = the mol fractions A, B, in the liquid at the condenser
xAN, xBN = the mol fractions A, B, in the liquid leaving the Nth stage (the pot)
αAB = relative volatility of components A, B,
For more complex systems, such as binary mixtures containing azeotropes or

those having significant non-ideal behavior, more complete calculations using the
McCabe Thiele diagram (Fig. 2) are required. In a binary system under total reflux the
operating line is the diagonal on the x-y diagram, and graphical stepping off theoretical
trays is shown in figure 1.
Figure 2 Example of Stage Calculation Under Total Reflux (Approximately 2.5

Theoretical Stages Shown)
50
page 51
3rd Theoretical Stage
Equilibrium Line
y (mole Distillate
fraction
more
volatile 2nd Theoretical Stage
component
in the vapor
phase)
1st Theoretical Stage
Operating Line
Bottoms
x (mole fraction of more volatile component in liquid)
The overall tray efficiency is defined the ratio

N
ηtray = 100
N actual
where N = the number of theoretical trays determined based analysis of feed, distillate
and bottoms
Nactual = the number of physical trays (does not include the reboiler)
ηtray = the tray efficiency
Perhaps the simplest correlation for predicting overall tray efficiency is that of O’Connell
(Fig. 1, Ref. 2 attached). A figure based on this is shown below, prepared by Lockhart
and Leggett.
51
page 52
Fig. 1 O'Connell Predictions of Tray Column Efficiency
from E.J. Henley, J.D. Seader, Equilibrium-Stage Separation Operations in Chemical

Engineering, Wiley, 1981
Procedure
The procedure for operating the Technovate column is found in the appendix. Students
must demonstrate that they have completed the distillation-training program on the
Virtual Chemical Engineering Laboratory before they will be permitted to work on
the distillation column.
1. After the column has operated steadily under total reflux with the controls on
automatic, sample both the distillate and the reboiler composition in five-minute
intervals. Take at least three samples of both distillate and reboiler.
2. Change the boil up rate by adjusting power and repeat step 1.
1. From overhead and still pot samples, calculate overall tray efficiency for the two
columns.
2. Show the McCabe-Thiele diagram for the experiment.
52
page 53
3. Compare the measured efficiencies with the Lockhart and Leggett version of the
O’Connell correlation.
4. Discuss the effect of preheating reflux.
References
1. McCabe, W. L. and J. C. Smith, Unit Operations of Chemical Engineering, 4th

ed., pp. 493-498, 507-510 (McGraw-Hill, 1985)
2. O’Connell, H. E., Trans. A.I.Ch.E., 42 741-755 (1946).
3. Ballard, L. H. and M. Van Winkle, “Vapor-Liquid Equilibria” I & E. C. J. 44,

2450-2453.
4. Bennett, C. O. and J. E. Myers, Momentum Heat and Mass Transfer, 3rd ed., pp.
658-662, 674-677, 723,763 (McGraw-Hill, 1982).
5. “Technovate Fractional Distillation System, Model 9079,”Technovate, Pompano

Beach, FL (in the Chemical Engineering Department office).
6. Hines, A. L. and R. N. Maddox, Mass Transfer, pp. 300-301; 444-449 (Prentice-Hall,

1985).
7. Henley, E. J. and J.D. Seader, Equilibrium-Stage Separation Operations in Chemical

Engineering, pp. 362-69, (John Wiley and Sons, New York, 1981).
8. Perry, R. H., Don Green and R. O. Maloney, eds., Chemical Engineering

Handbook, 6th ed. sec. 13. pp. 27-35 (McGraw-Hill, 1984).
JWH 7/28/93
CRN 3/30/96
JWH 1/7/99
CRN 7/21/99, 8/4/2
53
page 54
Appendix A
Isopropanol/Water at 760mm (from ref. 8)
Temperature Mole fraction isopropanol in
liquid vapor
100 0 0
97.57 0.0045 0.0815
96.2 0.0069 0.1405
93.66 0.0127 0.2185
87.84 0.0357 0.3692
84.28 0.0678 0.4647
82.84 0.133 0.5036
82.52 0.1651 0.5153
81.52 0.3204 0.5456
81.45 0.3336 0.5489
81.19 0.3752 0.5615
80.77 0.472 0.586
80.73 0.4756 0.5886
80.58 0.5197 0.6033
80.52 0.5945 0.633
80.46 0.788 0.7546
80.55 0.802 0.768
81.32 0.9303 0.901
81.85 0.966 0.9525
82.39 1 1
54
page 55
XY Diagram Isopropanol-Water
0.9
0.8
0.7
0.6
vapor
0.5
0.4
0.3
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
liquid
55
page 56
13. Batch Distillation, Constant Overhead Composition,

Technovate Column
Objective
To show the effect of controlling batch distillation by maintaining constant overhead

composition.
Apparatus

sieve trays, condenser, product accumulator/reflux drum, and pumps for
supplying reflux and product.
2. Factory Floor ™ and OPTO LCSX programmable logic controller (PLC).
3. Specific gravity bottle, refractometer or other appropriate analytical instruments.
Background
Maintaining constant composition of the product requires increasing the reflux

ratio as the pot composition changes. Figure 1 shows the McCabe Thiele diagram for
this distillation operation. Point xp1-3 represents the initial composition of the reboiler. As
the reboiler becomes depleted of volatile components, the composition moves to xp2-3 and
eventually, xp3-3. Graphically, operating lines of varying slopes are drawn from the
distillate composition. Then the number of theoretical plates corresponding to those in
the column is stepped off to determine the corresponding bottoms composition for each
reflux ratio.
56
page 57
Fig. 1 McCabe Thiele Diagram for Batch Distillation at Constant Composition
xAD
L/V1
L/V2
L/V3
xp3-3 xp1-3
xp2-3
The Bogart equation determines the time required for a distillation to produce a bottoms
product of a particular composition. It is an integrated material balance.
57
page 58
Mi ( yA D − xA i) xA i d xA
θ= ∫
V xA f ( 1 − ) ( yA D − x A ) 2
L
V
where L = the reflux flow rate (varies with xA)
Mi = the total number of moles initially in the reboiler
V = the vapor rate to condenser (constant)
xAi = the mole fraction of more volatile component initially in reboiler
xAf = mole fraction of more volatile component in reboiler at the end of the
distillation
yAD = the mole fraction of more volatile component in distillate (constant in our
case)
θ = time
The quantity distilled can then be determined from a material balance.

x Ai − x Af
Mi − M f = M
y AD − x Af
where Mf = the total number of moles in the reboiler at the end of the distillation
Control of Distillation at Constant Overhead Composition
Like most sophisticated pieces of equipment, the Technovate column requires a

process controller for successful operation. Maintaining a constant temperature at the top
of the column allows the column to provide constant distillate composition. Regulating
the amount of recycle returned to the column controls the temperature. Product is
removed from the receiver to maintain a constant liquid level in the receiver.
The OPTO LCSX programmable logic controller (PLC) provides the controllers
shown on Figure 2.
The temperature at the top plate of the column is measured by a thermocouple. A

Proportional Integral Derivative Controller (PID) controller in the program processes the
signal. The set point is set at the desired tray temperature corresponding to the
composition of the distillate. The control valve in the reflux line opens to provide more
reflux liquid as the temperature tends to rise above the set point.
Since the vapor rate V = R + D in the column is constant, any excess condensate
is taken as product D by maintaining the level in the receiver (accumulator) constant by
another PID Controller which maintained a constant level in the product receiver.
In most operations, the output of the PID controller would be directly converted to a
signal that is converted by a transducer to a pressure that controls the position of an
automatic valve. Thus, an output signal from the PID control of 60% would cause the
valve to open 60%. For a variety of technical reasons, this approach does not work on
the Technovate still. Therefore, the output signals of PID controllers go to timers. Each
timer has a cycle of 6 seconds. The fraction of the period during which the valve is open
58
page 59
is determined by the output of the PID controller. Thus, if the PID output signal is 60%,
the valve is open 60% of the size second period, or 3.6 seconds.
Fig.2 Schematic of the Technovate Still
Condenser
Feed Heater
Transducer
Column
Flowmeter
TC
DP
Transducer
OPTO22/PC
Pump
Set T Set Point
Reboiler Product Tank PID PID
Timer Timer
The computer will store reflux and product flow rates as distillation proceeds.
These signals are not shown in figure 2 to keep the figure simple. Additionally, you will
retain the product to measure its mass and composition. The reflux ratio will start at
some low value and increase to total reflux as the distillation continues. This ratio can be
calculated from the experimental data once they have been imported into a spreadsheet.
Ultimately, distillation would achieve total reflux; however, the liquid level in the
reboiler may drop to a very low level. When this occurs the reboiler turns off.
Procedure
The procedure for operating the Technovate column is found in the appendix. Students
must demonstrate that they have completed the distillation-training program on the
59
page 60
Virtual Chemical Engineering Laboratory before they will be permitted to work on
the distillation column.
General Procedure
1. Follow the procedure in the appendix to start the still and switch control to
automatic.
2. Withdraw about four samples from the reboiler and condenser during the
distillation (do not withdraw samples from the receiver) and analyze them. The
distillation process may proceed rapidly so you may have to work quickly.
1. Compare the measured bottom compositions with those predicted from a

McCabe-Thiele diagram for the tops samples taken during the distillation. You
will have to determine the reflux ration from the flow rates. Correct for the tray
efficiency determined previously to estimate the number of theoretical trays. A
sample McCabe Thiele diagram is shown in Fig.1.
2. Plot reflux ratio and reboiler and overhead temperature vs. time.
3. Using graphical or spreadsheet integration, estimate the time required for the
distillation from the Bogart equation. Compare to the actual time required.
References
1. McCabe, W. L., J. C. Smith and P. Harriott, Unit Operations of Chemical

Engineering, 4th ed., pp. 507-10, McGraw-Hill, New York, 1985.
2. Perry, J. H. D.W. Green and J. O. Maloney, Chemical Engineer’s Handbook, 6th

ed. sec. 13 pp. 27-35 and pp. 82-90 McGraw-Hill, New York, 1984.
CRN/art 8/4/93
JWH 1/07/99
CRN 7/19/99, 8/11/2
60
page 61
14. Batch Distillation at Constant Liquid Rate, Technovate Column
Objective
To demonstrate an understanding of distillation and the operation of process equipment

by operating the Technovate still to produce product using constant liquid rate control
scheme.
Apparatus

sieve trays, condenser, product accumulator/reflux drum, and pumps for
supplying reflux and product.
2. Factory Floor ™ and OPTO LCSX programmable logic controller (PLC).
3. Specific gravity bottle, refractometer or other appropriate analytical instruments.
Background
The background sections for experiments 12 and 13 describe the apparatus and
calculation details. A common method of batch distillation is reflux at constant liquid
rate. In this experiment, the boil up rate will be fixed by the power supplied to the
reboiler, the liquid rate will be held constant by setting the reflux valve to a constant
position, and maintaining a constant level in the accumulator will control the rate of
distillate removal. This method leads to the simplest control scheme but will cause the
composition to vary as the distillation proceeds.
Procedure
The procedure for operating the Technovate column is found in the appendix.
Students must demonstrate that they have completed the distillation-training
program on the Virtual Chemical Engineering Laboratory before they will be
permitted to work on the distillation column.
General Procedure
1. Charge the reboiler to about two-thirds full of a mixture stored in the hold tank.
Take a sample of this material for analysis. Bring to a boil under total reflux.
1. Follow the procedure in the appendix to switch control to automatic.
61
page 62
3. Withdraw about four samples from the reboiler and condenser during the
distillation (do not withdraw samples from the receiver) and analyze them. The
distillation process may proceed rapidly so you may have to work quickly.
4. Watch the tops temperature and stop when the temperature in the upper trays rises
to about 3 degrees above the temperature when you switched to automatic. The
temperature is a function of the amount of the less volatile component on the tray.
As distillation proceeds and the still is depleted of more volatile component, the
temperature in the upper section of the column will begin to rise.
4. Measure the amount and composition of the product.
1. Compare the measured bottoms compositions with those predicted from a

McCabe-Thiele diagram for the samples taken during the distillation. You will
have to determine the reflux ration from the flow rates. The calculation
procedure is described in experiment 16 and ref. 2. Correct for the tray efficiency
determined previously to estimate the number of theoretical trays. A sample
McCabe Thiele diagram is shown in Fig.1. of experiment 14
2. Plot reflux ratio and reboiler and overhead temperature vs. time.
3. Using graphical or spreadsheet integration, estimate the time required for the
distillation from the Bogart equation. Compare to the actual time required.
References
1. McCabe, W. L., J. C. Smith and P. Harriott, Unit Operations of Chemical

Engineering, 4th ed., pp. 507-10, McGraw-Hill, New York, 1985.

CRN 8/22/00, 8/4/2
62
page 63
15. Batch Distillation at Constant Reflux, Oldershaw Column
Objective
To demonstrate the effect of fractionating power on sharpness of the separation curve of

a batch distillation.
Apparatus
1. 1000 ml round bottom distilling’ flask, l0 tray Oldershaw column, reflux head,
condenser, and product accumulator/reflux drum,
2. Reflux timer
3. Heating mantle
4. Specific gravity bottles, refractometer, or other appropriate analytical instrument.
Background
In a continuous differential, batch distillation, a material balance on constituent A

gives
n1
dn x1 dx
∫ = ∫
n2 n x2 y − x
where n = the number of mols in the still pot

x = the mol fraction of the more volatile component in the still pot
y = the mol fraction of the more volatile component in the distillate
the subscripts 1 and 2 refer to the beginning and end of the distillation
If A is the more volatile constituent, x decreases as the distillation proceeds. If

there is only one equilibrium stage (the still pot), y is assumed to be in equilibrium with
x . The vapor composition can then be determined by a bubble point calculation or from
the y-x or T-x-y diagrams. This is the simple Rayleigh or differential distillation.
If a multistage fractionating column supplements the still pot, the number of

theoretical stages and the reflux ratio determines the relationship between y and x. In the
simplest consideration, at any instant the system can be considered as a steady-state
rectifying system with a slowly changing liquid composition, x, in the reboiler.
Two limiting cases are common; in practice the distillation is stopped when the
purity of the overhead product falls below a minimum specification:
1. Run at a fixed reflux ratio, letting the vapor composition (y) change as the liquid
composition (x) changes.
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2. Increase the reflux ratio as the fraction of volatile material in the liquid (x)
decreases to maintain a constant overhead composition (frequently indicated by a
constant overhead temperature).
Additionally, batch distillation is often performed at constant liquid flow (experiment

14).
This experiment will be run at constant reflux ratio as the simplest case for this
apparatus.
Procedure
1. Charge flask boiler about two-thirds full with a binary mixture containing about
30 mol percent of the more volatile constituent,
2. Prepare a calibration curve of composition vs. refractive index or specific gravity.
3. Bring system to a boil at total reflux and measure overhead and boiler
compositions.
4. From the compositions and the equilibrium relationship for the system, set a
reasonable target product composition, y, and a minimum reflux ratio to achieve
it.
5. Set a reflux ratio on the timer at about 1.2 times the minimum value and begin
product distillation.
6. Follow the product weight, instantaneous and average product composition, and
temperatures in reboiler and overhead.
1. Plot overhead temperature, T, and composition of product, y, versus the fraction
of the original charge remaining in the pot, n/n0. Compare with that for a simple
differential distillation based on the equation given above.
2. From the data at total reflux, estimate the overall tray efficiency.
3. For several points during the distillation, compare the compositions with those
predicted from a McCabe-Thiele diagram (corrected for the tray efficiency
determined in step 2).
4. Comment on the optimization involved in choosing a reflux ratio, that is, what
are you gaining or losing as you increase reflux ratio?
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References
1. Henley, E. J. and J.D. Seader, Equilibrium-Stage Separation Operations in
Chemical Engineering, pp. 362-69, (John Wiley and Sons, New York, 1981).

3. Oldershaw, C. F., “Perforated Plate Columns for Analytical Batch Distillation”,

Ind. & Engr. Chem., Apr. 15, 1941, pp. 265-268.
4. Collins, F. C. and Y. Lantz, “Evaluation of Laboratory Distillation Apparatus,”

Ind. & Engr. Chem., Vol. l8, No. 11, 1946, pp. 673, 675-677.
JWH
1l/6/85
rev. CRN
4/19/96
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16. Absorption in a Packed Column
Objective
To demonstrate an understanding of mass transfer by determining the liquid and gas
handling capacity of a packed tower and measuring rate of mass transfer in absorbing
carbon dioxide from an air/CO2 mixture.
Apparatus
1. Glass absorption column 102 mm (4 in.) in diameter packed to a height of
approximately 120 cm (4 ft) with ½ inch, ceramic, Intalox saddles, liquid
recirculating and metering loop; air and C02 metering and mixing; manometer for
measuring column pressure drop.
2. CO2 cylinder and regulator
3. Standard solutions and burettes for analysis of tower liquor.
Background
Flooding
A packed tower is a countercurrent-contacting device similar to a tray column in

that liquid flows downward by gravity and gas flows upward. However, it differs in that
normally, unlike the idealized stage operation, the phases are never in equilibrium and
the operating “line” is truly continuous. In addition, interfacial area for mass transfer is
produced by the flow of liquid over the packing material as opposed to the turbulent
action of bubbles churning through liquid as in tray columns.
The gas and liquid handling capacity of a column determines the diameter
required to do a certain job. The mass transfer rates determine its height. The two
factors interact in the economic choice of gas/liquid flow rates and L/G. If the gas flow
rate to a column is increased while the liquid flow is held constant, the pressure drop will
increase as G0.8 up to a point that the quantity of water (i.e., the film thickness on the
packing and in channels) starts to build up. Above this “loading point” pressure drop
increases more rapidly until at the “flood point” the column fills with liquid, pressure
rises very rapidly, and liquid is spewed out the top of the column.
The flooding correlation shown below gives the most widely used correlation for
flood point and pressure drop for flows at less than flooding conditions. A similar graph,
provided by the manufacturer of the packing used in the experiment, Norton Co., is
attached.
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Fig. 1 Flooding Correlation
from James R. Welty, Charles E. Wicks and R. E. Wilson, Fundamentals of Momentum,

Heat, and Mass Transfer, 3rd ed., Wiley, 1984
Mass Transfer
Mass transfer takes place through both gas and liquid films. In dilute solutions,
the effect of the fact that only one component in the gas phase is diffusing during an
absorption process can be neglected. The rate of mass transfer, dNA (kgmols/hr) in a
small element of height of tower (dz) is given for the gas a liquid phases respectively by
dN A = k y ( y − yi ) a w dz
(1)
dN A = k x ( xi − x) a w dz
where a = wetted area of packing (ft2/ft3)

ky, kx = mass transfer coefficients for mole fraction driving force, (lbmole/hr ft2)
y, x = mole fractions of material being transferred, in the bulk of the gas and
liquid
phases, respectively
xi, yi = mole fractions of material being transferred on the opposite sides of the
interface. When yi is in equilibrium with xi and Henry’s law holds
yi = (H/P)xi,
where H = Henry’s law constant and P is the total pressure; this is often written
yi = mxi;
where m = the local slope of the equilibrium curve.
Data for the CO2/water system are found in Reference 3 and are attached.
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By a material balance on the two phases and integrating (see Eqs. 23-19 and 23-20,
McCabe & Smith and Eqs. 35-15 and 35-17, Bennett and Myers), the column height ZT
can be found:
G my yb
dy
ZT = ∫ (2)
k ya w ya y − yi
G mx x b dx
or ZT = ∫ (3)
k xa w x a xi − x
where Gmy and Gmx = the molar mass velocities of the gas and liquid phases (lbmol/hr
ft2), based on the empty column.
In more concentrated gas mixtures, the denominator of the integral of equation

(2) should include the correction for the fact that only one constituent is diffusing: (1-y)L
or log-mean mole fraction of the carrier gas.
For convenience in correlating ky and kx it has become customary to express the

transfer capability as “height of a transfer unit”, H(or HTU).
G my
Hy = (5)
k ya w
G mx
Hx = (6)
k xa w
Probably the most up-to-date correlation of mass transfer data in packed columns is that
of Bolles and Fair (attached). Note that notation differs slightly from that of McCabe
and Smith.
Since the interface composition cannot be measured directly, the concept of overall
driving forces and mass transfer coefficients has been introduced:
dNA = Kx(x*-x) = Ky(y-y*)
where y* and x* are gas and liquid phase compositions that would be in equilibrium with
the bulk composition of the other phase:
y*=mx and x*= y/m
The overall coefficients are related to the film coefficients by the additive resistance
concept. For example
1/Kx = 1/mky +1/kx
Hox = Hx + (Gmx/mGmy)Hy
For the absorption of gases of low solubility, such as CO2 or O2 into water the
mass transfer rate is controlled by that in the liquid phase. Thus, the experimental data in
the tests should be used to calculate Hx (HL in Bolles/Fair terms) or kx (kL).
For dilute phases and straight equilibrium curves integration of the overall
coefficient analogy of Eq. (3) and substitution of the definition of Hox gives
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( xb* − xb ) − ( x a* − x a )
( x − xa ) ( x * − x ) lm =
Z T = H ox *b and ( xb* − xb )
( x − x) lm ln *
( xa − xa )
or ZT = Hox Nox
where Nox = the “number of overall liquid phase transfer units”.
Absorption into an alkaline carbonate/bicarbonate or amine solution would increase rates
of absorption and would more nearly represent an industrially significant case. The
mathematics is treated in Welty, Wicks, and Wilson.
General Procedure
1. With no liquid being fed to the column, determine a curve of pressure drop per
unit height as a function of gas rate up to maximum gas flow permitted by the
flow meters. Use air alone.
2 Repeat using water flows corresponding to 1000 lbm/hr ft2 as a start and doubling
each time to a maximum of 16,000 lbm/hr ft2 or as high as the flow meter will
allow, whichever is smaller.
Maintain running plots of pressure drop and identify flooding points, but do not
allow packing to be agitated severely or ejected from the column at flood.
3. Adjust water flow to midrange (about, 4000 lbm/hr ft2) and air rate to provide a
pressure drop of about 0.5 in. H2O/ft of packing. Take a sample of the effluent
water from the small valve near the water outlet by running it into an aliquot of
dilute NaOH and excess BaCl2 to minimize loss of free CO2 Turn on CO2 supply
and adjust flow to about two-thirds rate on the small rotameter. After about 10
minutes, take another sample of the tower effluent.
NOTE: The NaOH is approximately 0.1N. The preliminary report should
consider what the best concentration of HCl should be considering the solubility
of CO2
4. Titrate with 0.1 N HCl to phenolphthalein end points to determine CO2
concentration plus any fixed bicarbonate in the incoming city water. Free CO2 is
taken as the difference between the carbonate content of the incoming and
effluent water.
5. Repeat at two or more higher liquid rates.
1. Compare your measurement of the flood point with that of Eckert (Fig. 35-12,
Bennett and Myers or Fig. 31-22, Welty, Wicks and Wilson).
2. From the flow rates, measured change in CO2 content of the liquid stream, and
inlet concentration of CO2 in the gas stream calculate
a) the outlet concentration of CO2 in the gas stream
b) the mean driving force for the liquid phase transfer
c) NoX and HoX
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3. Compare results with the correlation of Bolles and Fair (their Eq. 14) or other
references. Use the calculated flood point if agreement in part 1 was poor.
Consider Intalox saddles equivalent to Berl saddles.
4. Compare results with Eq. 34-12, Bennett and Myers, given below.
η
 L
H L = φ  Sc 0.5
 µ
where Sc = the Schmidt number

L = the liquid rate (lb/hr ft2)
µ = the viscosity of the liquid phase (lb/ft hr)
φ and η are constants determined from the table below
Constants for determining HL
Type of Packing φ η Range of L
Rashing rings
3/8 inch 0.0018 0.46 400-15,000
1 inch 0.010 0.22 400-15,000
2 inch 0.012 0.22 400-15,000
Berl Saddles
1/2 inch 0.0067 0.28 400-15,000
1 inch 0.0059 0.28 400-15,000
1 ½ inch 0.0062 0.28 400-15,000
source: Bennet & Myers p. 589
References
1. McCabe, W. L., and J. C. Smith, Unit Operations of Chemical Engineering, 4th
ed., pp. 617-631 and 637-641 (McGraw-Hill, 1985).
2 Bolles, W. L. and J. R. Fair, Chemical Engineering, July 12, 1982, p. 109.
3. Perry, R. H., D. W. Green and J. O. Maloney eds., Chemical Engineer’s
Handbook, 6th ed., sec 3, p. 101 McGraw-Hill, New York 1984.
4. Bennett, C. O. and J. E. Myers, Momentum. Heat. and Mass Transfer, 3rd ed., pp.
541-547 and Ch. 35 (McGraw-Hill, 1982).
5. Hines, A. L. and R. M. Maddox, Mass Transfer, Ch. 12 and Table 8-6, p. 508
(Prentice Hall, 1985).
Appendix 1
Table 3-125 Carbon Dioxide
Total Weight CO2 per 100 weights H2O
pressure,
atm
12C 15C 25C 31.04C 35C 40C 50C 75C 100C
25 ... 3.86 ... 2.80 2.56 2.30 1.92 1.35 1.06
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50 7.03 6.33 5.38 4.77 4.39 4.02 3.41 2.49 2.01
75 7.18 6.69 6.17 5.80 5.51 5.10 4.45 3.37 2.82
100 7.27 6.72 6.28 5.97 5.76 5.50 5.07 4.07 3.49
150 7.59 7.07 ... 6.25 6.03 5.81 5.47 4.86 4.49
200 ... ... ... 6.48 6.29 6.28 5.76 5.27 5.08
300 7.86 7.35 ... ... ... ... 6.20 5.83 5.84
400 8.12 7.77 7.54 7.27 7.06 6.89 6.58 6.30 6.40
500 ... ... ... 7.65 7.51 7.26 ... ... ...
700 ... ... ... ... ... ... 7.58 7.43 7.61
See also Table B-6, p.508, Ref. 5.
JWH/KMM/nn 3/22/91
CRN 5/2/96
JWH 4/2/97 1/07/99
CRN 8/4/2
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18. Mass Transfer in an Agitated Tank
Objective
To demonstrate understanding of the mixing process by determining the effect of

agitation intensity on the rate of solution (time to dissolve) rock salt in agitated tanks and
recommend a scale up method.
Apparatus and Reagents
1. Chemineer agitation assembly, with strain gage or torque measurement and

tachometer.
2. Yellow Springs Instrument solution conductivity indicator with plastic

conductance cell.
3. Set of screens (Ro-Tap shaker may be used for screening)
4. Rock salt
Background
Mass transfer coefficients to bubbles and other suspended materials in stirred

tanks are functions of agitator type and speed, particle size and density among other
factors. The dissolving rate will change as the surface area of the particles decreases and,
in batch systems, as the concentration of salt increases in the solution.
Mass transfer coefficients can be estimated from the concentration history in the
tank. The salt concentration can be determined from the solution conductivity. The
following set of equations can be used to model the process:
WA = kA(Csat-C) = Vt(dC/dt)
A = n(4πr2) dr/dt = WA/ρA
where WA = rate of mass transfer, kg/s
k = mass transfer coefficient, m/s
A = surface area of all n particles of radius r and density
ρs, m 2
Csat, C = concentration of salt at the surface and in
solution, kg/m3 Vt = Volume of solution in tank, m3
The initial particle radius is obtained by screen analysis of the charge; n is estimated
from the charge weight M = nρs4πr3/3 and is assumed to be constant during the run. A
spreadsheet numerical integration can simulate the run and calculate k and r from the
concentration vs. time data.
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General Procedure
1. Develop a calibration curve of the solution conductivity as a function of salt

concentration at room temperature, which is recorded.
2. Screen to a sharp cut enough salt to prepare several (minimum 6) batches of 0.5-1
wt% salt solutions in the tanks. You must estimate the amount of salt required.
Prepare salt at two different mesh sizes.
3. Make four runs in each tank using a different (over as wide a range as possible)
impeller speed for each run. For each run measure concentration at various times.
Pump out the tanks and refill with fresh city water between runs.
4. Repeat for a different particle size.
1. Develop a set of dimensionless groups that might be used to correlate the data.
2. From plots of dissolving rate as functions of impeller speed (RPM), tip speed
(m/sec) power/volume ratio (W/m3), etc. recommend a method of scale up.
3. See if the dimensionless groups are useful in correlating aids for your data.
4. Estimate the mass transfer coefficients at several stages of the solution process
and compare the results with what looks reasonable from the literature (e.g. Ref.
5).
References
1. MaCabe, W.L., J.C. Smith, and Peter Harriot, Unit Operations in Chemical
Engineering, 4th ed. Ch. 9 pp. 604-5, McGraw-Hill, N.Y. 1985.
2. Levenspiel, Octave, Chemical Reaction Engineering, 2nd ed., pp. 369-71, Wiley,
N.Y. 1972.

JWH
1990 4/2/97 1/077/99
rev. CRN 5/3/96 8/4/2
73
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19. Fluidization
Objective
To demonstrate an understanding of fluidization by measuring the properties of a packed

bed under fluidized conditions. Specifically, to calculate the value of the exponent n in
the fluidization equation.
Background
Fluidization occurs when the velocity of a fluid in a continuous phase is sufficient

to lift an unrestrained bed of solid particles. The minimum velocity for this to occur is
called a minimum fluidization velocity. At velocities higher than the minimum, the bed
expands. This expansion is correlated by the following equation:
n
 h 
V = Vt 1 − 0.55 r 
 h 
where h = the height of the bed of particles when the superficial velocity is V
hr = the rest height of the bed of particles
V = the superficial velocity of the water defined as the volumetric flow divided
by
the cross sectional area of the tube.
Vt = the terminal velocity of a single particle
Fluidization is a key to unit operations in such technologies as:

1. Catalytic cracking of gas oil to gasoline
2. Polymerization of propylene to polypropylene
3. Cell immobilization and production of biomolecules
General Procedure:
Part 1: Drop Test in Vertical Tubes (Room 119/120)

1. Fill the vertical tube to the mark with water at room temperature.
2. Pick 40 particles of polystyrene and drop them one at a time into the vertical tube
filled with water. Measure the fall time.
3. Calculate the velocity. Calculate the mean, variance and 90% confidence interval
for these data.
4. Using the average terminal velocity, Vt, and Stokes law, calculate the effective
diameter. Using the Reynolds number, verify that the velocity is in the Stokesian
region, if it is not, recalculate the effective diameter.
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Part 2: Bed Fluidization (Room 127)
1. Record the height of the bed of particles at rest.
2. Turn the valve slowly and slowly lift the bed. When stable, note the flow rate.
3. Repeat this process 10 times or more, each time noting the height and water flow
rate.
1. Use the measured values of the velocity and height to calculate the value of n.
2. Average these values and calculate an average n for your experiment.
GJM 1992
rev. CRN 5/3/96, 8/11/2
75
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20. Filtration
Objective
To demonstrate an understanding of the filtration process by measuring the properties of

an incompressible filter cake by estimating the size of a belt filter to filter this slurry on a
production scale.
Apparatus
1. Filter (test filter, Multi-Metal Wire Cloth, Inc.

2. Vacuum flask
3. Vacuum gauge
4. Aspirator
5. Solids (e.g. talcum powder)
Background
Generally, industrial filters are of three main types: plate and frame, drum and
horizontal belt filters. The type of filter used depends upon solids loading of the input,
the nature of the filter cake, the specific gravity of the solids relative to the fluid and
desired solids concentration of the filtrate. Additionally, filtration can be done under
vacuum or pressure.
Fig. 1 Plate and Frame Filter
Fig. 2 Drum Filter
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Fig. 3 Horizontal Belt Filter
The scale up of filtration of incompressible (that is, cakes composed mainly of solids that
are not swollen by the filtrate) cakes is relatively straightforward. Simple bench scale
tests can often yield good data for a preliminary design using an apparatus that looks
somewhat like a modified filter used in chemical laboratories.
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The derivation of the design equation is straightforward. Consider a filter cake as
shown in the figure 4.
Fig. 4 Schematic of Filtration
Slurry flows through the cake and cloth driven by the pressure difference between
the top of the cake (P0) and the bottom of the cloth (P1). The liquid flow is laminar
through the pores of the cake and cloth; therefore, the flow rate per unit area of filter is
proportional to the pressure difference (P0 - P1). This yields the following equation.
d ( V / A ) ∆P
= (1)
dt R
where A = area of filter.(m2)

V = the volume of liquid that passes through the filter (m3)
R = the resistance to flow, a function of the cake, cloth and slurry
∆P = P1 -P0 = the pressure difference (kPa)
Consider, now, the resistance to flow caused by the filter cake and the filter cloth.
Assume that these two materials each contribute to the overall resistance to flow. Then R
can be written as
R = Rcloth + Rcake (2)
where Rcloth = the resistance of the cloth to flow of the fluid

Rcake = the resistance of the cake to flow of the fluid
If we further assume that the cloth is not "blinded" (the pores of the cloth are not plugged
with solids so that flow is restricted), then Rcloth will not change during the course of the
filtration operation and is a constant for the cloth and fluid. Furthermore, solids tend to
form cakes which are homogenous throughout and which do not compress as the cakes
thicken. Such filter cakes are called incompressible. For such cakes, the resistance to
flow is proportional to the thickness of the cake. Thus, we obtain
R = Rcloth + kh (3)
where k' = the constant for the cake

h = the height (or thickness) of the cake
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page 79
Substituting equation 3 into equation 1 yields
d (V / A) ∆P
= (4)
dt R cloth + kh
It is convenient to take the inverse of this equation when treating experimental data
1 R kh
= cloth + (5)
Q ∆P ∆P
where Q = the volumetric flow rate per unit area (m3 filtrate/m2 filter surface/min)
This equation tells us that the inverse of the flow rate will be a linear function of the cake
thickness.
General Procedure
1. Setup apparatus and prepare a slurry of 5 wt% solids.
2. Measure the filtration constants for the filter and filter cloth and determine if your
slurry was indeed incompressible (reading the background section should provide
you with a suggestion as to how to prove that).
3. Plot the size of a belt filter filtration area vs. cake thickness for a filter designed
to filter 20 tons/hour of dry cake from a 5 wt% solution. Assume the filter
vacuum is the same vacuum obtained in the laboratory.
References
1. Bennet, C.O. and J.E. Myers, Momentum, Heat and Mass Transfer, 3rd ed.,
McGraw-Hill, New York, N.Y., 1982, Chapter 18 especially note the derivation
and theory of equation 15-23 p. 233.
2. McCabe, W.L., J.C. Smith, and Peter Harriott, Unit Operations of Chemical
Engineering, 4th ed. Pp. 870-886, McGraw-Hill, New York, N.Y., 1985.
79
page 80
Appendices
80
Startup and Operation Procedure for the Technovate Still
Note: sampling procedure and times are described in the Experiments
Background
The Technovate still was purchased in 1981 and has undergone a series of upgrades. The
most recent upgrade, completed in the summer of 2000, included the addition of an
OPTO 22 LCSX programmable logic controller (PLC) and the writing of the necessary
control software. A Pentium class computer using Factory Floor software drives the
LCSX.
The distillation column is easily the most expensive and complex single piece of
equipment in the undergraduate lab. Computer control of the distillation column is
essential for its operation. Care must be taken when running the column to ensure both
safety and accuracy of results. Students must read and follow the startup procedure
given below. Failure to do so may result in removal from the lab and failure of the
course.
Each instruction contains information about what is to happen after you have
successfully completed it. If the system responds differently, consult the instructor
before proceeding.
A. Preliminary Preparations.
1. Turn on the power to the still by throwing the “Main Power” switch located in the
center front of the still. Only the red light above this switch should be
illuminated. If any other lights are come on, turn off the switch below them.
2. Check the air trap for water, if there is water in the trap empty it. The air trap is
located behind the still, about halfway up and in the center. It is black with a
clear plastic bottom and a pressure gauge. Empty water by pushing the black
bottom piece to one side while holding a collection beaker under it. You should
see the water in the trap drain into your beaker
3. Turn on the air supply to the controllers. The air supply valve is located behind
and above the still. The pressure gauge on the trap should read 20 psi.
4. Turn on the computer by pressing the orange switch located behind the printer.
This switch also turns on the PLC. The computer should start. Once Windows
has completed its startup, launch the computer’s display program. Under
“Start\Programs”, open “Opto 22\OptoDisplay\OptoDisplay Runtime”.
OptoDisplay Runtime should open and load the still software. A schematic of the
still should appear. If the still schematic does not appear, you must load the
program (step 5). If it does appear, skip to step 6.
NOTE: Do not open any Opto applications other than the ones you are instructed
to. The applications for creating and modifying the OPTO software are included
on the computer for the convenience of the instructor. Students are not permitted
to modify or tamper with the OPTO programs or the computers. Violations of
this rule can result in immediate removal from the lab and failing of the course.
5. Load the still display program. In the OptoDisplay Runtime menu open
“File/Open Project”. The still display is in C:\Opto2\OptoDisp\Examples\\Still
and is named “Still”. Find the file and click on it to load it. A schematic of the
still should appear.
6. Turn the controller on by going to the “Start\Programs\Opto

22\OptoUtilities\OptoTerm” menu and clicking the left mouse button. A window
labeled “Opto Term” will appear.
7. In the white box on the OptoTerm dialog click “ChELab2”. The words ChELab2
will be shown in blue. On the OptoTerm menu click “Tools/Start Terminal. A
larger window labeled “ChELab2 – Terminal” will appear.
8. This program allows direct communication to the OPTO PLC in the white box,
notice the “>>” prompt. Type “_RUN” (do not include the quotes). Be sure to
use upper case. Press “enter”. Close the terminal and OptoTerm. The
temperatures on the schematic should now be reading about 20.
9. The computer software is equipped with audio alarms. These alarms will alert
you of situations that will require operator action when the still is in automatic
mode. You should verify that the audio alarms are turned off. Open the
“Alarms” window in OptoDisplay Runtime by selecting the “Window” menu
option. Select “Alarms” from the list of windows. If “Alarms” is not listed,
select “open” and select alarms from the list.
10. You have now turned all the equipment on.
B. Draining and Filling the reboiler
1. Check the liquid level in the reboiler, if the level is low, or if the column has not
been recharged since it was last used in the production mode, you will have to
drain the column. If you do not have to drain the column, skip to step 5. You
may check the level by checking the sight tube on the side of the reboiler. The
reboiler is the large aluminum covered device directly underneath the column.
2. Open the manual drain valve behind the reboiler. DO NOT open the drain valve
directly under the reboiler because this can cause material to spill.
3. On the controls in the front of the still, put the drain switch to open. The drain
switch is directly under the boiler power switch. You should hear a relay and the
light above the switch should come on.
4. Wait until the tank has drained as indicated by the level in the sight tube. Then
close the manual drain valve and move the drain switch to “Auto”.
5. Connect the feed line to the reboiler. The feed line is the long tube that passes
through the still panel near the top of the column. A quick connect fitting is at
the end. Attach the quick connect to the reboiler connection. Pull back on the
outer ring on the quick connect, while holding the outer ring back, slide the quick
connect over the male fitting on the top of the reboiler. Release the outer ring.
You should hear the quick connect lock. Pull on the quick connect to check that
it has properly seated. It should not pull off the male connector.
6. Open the automatic feed valve. On the OptoDisplay Runtime menu, select
Window\Manual Valve Control. A small, dark green window will appear. This
window allows you to control the automatic valves when the computer is in the
“Manual” mode. Valve position is described by a number from 0 (closed) to 100
(open). Move the mouse cursor to the number next to “Feed”. A rectangle
should appear around the number. Click the left mouse button. A small dialog
box label Send Value will appear. Type 100 (corresponding to open) and click
the OK button. The dialog box will close and the number 100 will appear next to
Feed. You may hear the valve open. The feed valve is now open.
7. Turn the feed pump on. The feed pump switch is located on the left of the row of
switches on the front of the still. You should hear the pump and liquid flowing
into the still.
8. Fill the reboiler until there is only about 2 inches of air left in the sight tube
located on the left of the reboiler.
9. When the reboiler is filled, turn off the feed pump and disconnect the feed line.
Disconnect the feed line by pulling back on the outer ring and sliding the quick
connect off the reboiler connection.
10. You have now filled the reboiler.
C. Starting the distillation column
1. Turn on the condenser cooling water. The valve is located on the wall behind the
still. A green hose runs from the valve to the still. Set the flow so that the condenser
rotameter reads between 0.5 and 1. The condenser rotameter is located on the front
of the still, to the right of the condenser.
2. Verify that the Feed and Reflux pumps are turned off by checking the lights above
their switches on the column. Also, verify that the manual drain valve behind the
reboiler is shut.
3. Turn the reboiler power on. The reboiler power switch is located below and to the
right of the main still power switch. Red lights above the reboiler switch and the
“Boiler Temp.” light should go on.
4. Adjust the boiler power to about 10 amps. The control to adjust reboiler power is
located just below the “Boiler Temp.” light. The ammeter is located to the left of the
main power switch and is labeled “AC amperes”. Adjust the knob until the ammeter
reads 10 amps.
5. Drain the accumulator to a level until it has no more than about 1 inch (about 10 on
the “Still Conditions” screen). This minimizes accumulator hold up for batch runs
and allows time for actions when condensation begins. If the accumulator is already
at this level, skip to step 10.
6. Open the product line to the feed tank. The feed tank is the orange tank behind the
still panel on the base of the still. The feed tank valve is directly above it. Open this
valve and shut the valve to the product line. The product line is the line with a plastic
hose.
7. Turn on the reflux pump. The switch is located next to the feed pump switch on the
front panel. You should hear the pump and see recycle from the pump flow into the
accumulator. The pump is somewhat oversized.
8. Open the “Manual Valve Control” window. Follow the procedure in step 6 of filling
the column only select the number next to “Product”. Open the valve following the
method in step 6 of “Draining and Filling the Reboiler”. Adjust the product
rotameter so that the flow is no greater than about 150 mL/min.
9. When the accumulator level is 1 inch or less shut off the reflux pump buy turning off
the Reflux pump switch.
10. Check that all the valve settings in the “Manual Valve Controls” window are set to 0.
If they are not 0, set them to 0 by following the procedure in step 6 of “Draining and
Filling the Reboiler”
11. Zero the product integrator in OptoDisplay Runtime by moving the mouse cursor
over the yellow word “Zero” in the still conditions window. The product should read
0
12. Switch the PLC to “Total Reflux”. On the “Still Conditions” screen, press the black
button next to the words “Total Reflux”. Open the “Total Reflux Control” window.
13. The controllers have two modes of operation “Manual”, in which you set the signal to
the valve and “Automatic”, in which the controller sets the valve. The letter “M” at
the bottom of the controller should be yellow, indicating that the controller is in the
manual mode. If the “M” is not yellow, move the mouse cursor over it and click the
left mouse button.
14. Set the controller output to 0. Controller outputs are scaled from 0 (closed) to 100
(fully open). Set the controller by moving the mouse cursor to the YELLOW
numbers next to “Valve”. Yellow denotes values you can adjust from the computer.
When a rectangle appears around the number, click the left mouse button. A dialog
box will appear. Enter the number 0 in the box and click “OK”. A 0 will appear at
the value you entered. DO NOT ATTEMPT TO ADJUST THE PID SETTINGS.
15. Setup to watch the temperatures as the column heats. Several temperatures are
displayed on the upper graph of the main screen of the Stills program. All the
temperatures are displayed on the schematic of this screen. A more complete
graphical display can be found by opening the “Temperatures” window. Open the
“Temperatures” window by selecting the “Window” option from the OptoDisplay
Runtime menu and selecting “Temperatures”.
16. Verify that the total reflux controller is in Manual mode and the output is set to 0.
Open the “Tot Reflux Control” window. The YELLOW numbers to the right of the
word “Valve” should be 0 and the Letter “M” should be yellow.
17. Wait. Heating the reboiler should take about a 30 to 45 minutes. DO NOT LEAVE
THE STILL UNATTENDED DURING THIS TIME.
18. When the tops temperature (T5) reaches 50C, turn the reboiler power to 7.5 amps by
adjusting the “Boiler Temp;” knob.
19. Turn on the reflux pump. The switch is located next to the feed pump switch on the
front panel. You should hear the pump and see recycle from the pump flow into the
accumulator. The pump is somewhat oversized. To prevent overpressure in the lines
when there is no flow, the pump recycles liquid back to the accumulator.
20. Open the “Levels and Flows” window. This window displays graphs of levels and
flows for the past fifteen minutes. Set the vertical axis to the accumulator level. At
the bottom of the graph is a button with a downward pointing arrow. Click the
button. A key showing the identities of the lines will appear. Move the mouse cursor
over the word “Accumulator” and click the left mouse button.
21. Allow the level in the accumulator to rise to about two inches (about 20 on the “Still
Conditions” screen) Set the Level Control valve setting to 20 –30. This setting is on
the Controller located on the “Total Reflux Control” window. Move the cursor to the
YELLOW numbers after the word “Valve”. Click the left mouse cursor when the
rectangle appears. Enter the number 20 in the dialog box and click “OK”.
22. Manually adjust the “Valve” setting (the yellow number to the right of the word
“Valve”) until the input stays approximately constant. (It will normally fluctuate +/-
0.3 due to signal noise.
23. When the level has been held constant in the manual mode for about 5 minutes,
switch the control to manual. FIRST, enter the set value equivalent to the current
input. Enter this value as you did the output signal to the valve. The new set point
will appear in yellow. SECOND, switch the controller to automatic by moving the
mouse cursor to the “A” and clicking the left mouse button. The A should turn
yellow. The M should turn black (indicating automatic mode) and the output signal
to the valve will turn yellow, indicating that you may no longer set this value. This
will cause the controller to maintain a constant level in the accumulator at its current
level. The output signal and the valve open time should now fluctuate.
24. Wait several minutes to verify that the controller is smoothly adjusting level. If the
controller opens the valve wide or shuts it completely, return the controller to
manual, set the output to a reasonable value and repeat steps 18 – 19. Note: it may
take several tries to switch to automatic.
25. The controller software is equipped with audio alarms that are triggered by events
that may require direct operator action. Enable these alarms by opening the
“Alarms” window and clicking the left mouse button when the cursor is over the
word “On”.
26. Turn on the reflux preheater. The reflux preheater switch is located next to the
“Boiler temp” knob on the still front panel. Set the dial to about 8. Both lights over
the dial should come on. The light on the left indicates that the reflux preheater is
activated. The light on the right indicates that power is actually going to the
preheater. There is an automatic cutoff to the preheater to protect it from
overheating. The light on the right may go out briefly but should, in general remain
on. Ad just the knob carefully to bring the reboiler feed to within 4 degrees of the
tops temperature.
27. You are now running the still under total reflux. This operation can continue
indefinitely.
C. Batch Distillation, Constant Flow
1. Begin by starting the column and running it under total reflux under automatic
control for about ten minutes so that the system can line out.
2. Place a large (1 L or greater) beaker on the floor in front of the still, in the
indicated area marked with yellow tape. Place the end of the hose in this beaker.
3. Verify that the product line valve is open and the valve to the product tank is
closed. These valves are located just above the feed tank, which is the orange
tank behind the still panel on the floor of the apparatus.
4. Zero the Product integrator on the PLC. This integrator estimates the total
product by integrating the flow over time. The value is shown on the “Still
Conditions” window. Zero the value by moving the mouse cursor over the
yellow word “zero” and clicking the left mouse button. DO NOT ZERO THE
INTEGRATOR WHILE YOU ARE DISTILLING PRODUCT.
5. Turn off the audio alarms by opening the “Alarms” window, moving the mouse
cursor over the word “off” and clicking the left mouse button. The word “off”
should turn yellow.
6. Open the window labeled Constant Reflux Flow. If the window is not in the list
under the “Windows” menu option, you can find it by selecting Open from the
“Widows” menu option of OptoDisplay Runtime. Verify that the controllers for
Constant Reflux Flow are in manual (The letter M should be yellow). If they are
not place the controllers in the manual mode by moving the mouse cursor to the
letter M and clicking the left mouse button.
7. Activate the Constant Flow Controllers by clicking the black button next to
“Batch, Constant Flow” on the “Still conditions screen. You have now switched
to the Constant Flow controllers.
8. Set the product set point to the current input value. Set the Reflux Flow Valve
setting to about one half its current value and place the product controller on
automatic. Adjust these settings as you did with the Total Reflux controller
9. Immediately reduce the power to the reflux preheater by about one unit on the
dial. Watch the reflux temperature to ensure that it does not exceed the
temperature on the top of the column (T5). You are now making product. This
operation will continue until either 1) sufficient material has been removed so
that distillation ends, or 2) the reboiler level drops causing the automatic cutoff to
shut it down, or 3) you shut the still down because you are out of time. In
general, the product flow should slowly decrease with time.
10. Place the Product controller on automatic by moving the mouse cursor over the
“A” for that controller and clicking the left mouse button. You may leave the
reflux controller on manual.
11. Turn the audio alarms on by opening the “Alarms” window, moving the mouse
cursor over the word “On” and clicking the left mouse cursor. The word “on”
should turn yellow.
12. As distillation proceeds, you will have to slowly increase the preheater power to
keep the feed temperature within 5 degrees of the tops temperature (T5). In any
event, do not draw more than 10 amps on the AC ampere gauge.
13. You are running the still while maintaining constant reflux flow.
14. Stop the distillation when the tops temperature T5, reaches about 85 degrees.
Batch Distillation Constant Temperature
1. Begin by starting the column and running it under total reflux under automatic
control for about ten minutes so that the system can line out.
2. Open the “Constant Temperature” window by selecting the “Window” option. If
the “Constant Temperature” window is not in the list of opened windows, select
“Open” and select “Constant Temperature” from the list. It may take a few
seconds for the window to start displaying values.
3. Verify that the controllers in the “Constant Temperature” window are in the
Manual mode. The M for each controller should be yellow. If they are not, move
the mouse cursor over the “M” and click the left mouse button.
4. Turn the audio alarms “off” by moving the mouse cursor over the word “Off” on
the “Alarms” window.
5. Switch to the “Constant temperature” mode by clicking the black button next to
the words “Batch, Constant T”. The button should turn red.
6. In the controller labeled “Temperature” enter the desired control temperature.

Reduce the valve setting to about one half its current value. Enter a value of 0 for
the YELLOW number by the word “Valve”
7. Reduce the preheater power by turning the control knob about one half unit
8. Gradually reduce the reflux flow and the reflux preheater until the temperature
rises to the desired operating temperature. You may also have to increase the
reboiler power.
9. When the still tops is at temperature switch the temperature control to automatic.
Make the set point of the product control the current setting and switch the
controller to automatic.
10. If the controllers attempt to extremely close or open the valves, switch the
controller back to manual, line it out manually and reattempt to switch to
automatic mode. It makes take several attempts to switch to automatic.
11. You are now performing a distillation while maintaining at constant tops
temperature. For a binary distillation, this should be equivalent to maintaining a
constant composition at the tops.
12. Distillation will continue until 1) breakthrough will occur and the tops
temperature will start to rise dramatically, 2) the reboiler level drops to a point
where the automatic cutoff turns off the reboiler power, 3) no more product is
collected, or 4) you shut down the still
Normal Shutdown from making product.
1. Turn the audio alarms “off” by moving the mouse cursor over the word “Off” on
the “Alarms” window and clicking the left mouse button.
2. Switch the product valve to Manual and set the controller output to 0. This closes
the product valve.
3. Set the reflux controller to manual and set the valve to about 50
4. Follow the steps for Normal Shutdown From Total Reflux
Normal Shutdown From Total Reflux
1. Turn off the reflux preheater and allow it to cool to 60 C. Wit is possible to
overheat the preheater causing damage to it. Therefore, it should be cooled
before the distillation process is stopped.
2. When the reflux preheater temperature is <60 C, turn off power to the reboiler.
3. About one minute after turning off the reboiler, shut off the reflux pump and
return the PLC to the Manual mode by clicking the black button next to the word
“Manual” on the “Still Conditions” screen.
4. On the “Still Conditions” window, switch the mode to manual by moving the
mouse cursor over the black button next to the word “Manual” on the “Still
Conditions” screen and clicking the left mouse button
5. When no more material is coming from the condenser, turn off the cooling water.
The valve is on the wall behind the still
6. Turn off the air to the still. Shut off the main power switch for the still.
7. Exit OptoDisplay Runtime. The history files of your run will be found in the
C:\Cdrom\Opto22\OptoDisp\Examples\Still folder. Your files will have the
names Rd000mmdd.*** where mm = the month, dd= the date and *** are the
extensions (there will be at least two). These files are in ASCII and can be
converted by Excel to a spreadsheet. The files may be large and you should zip
them before attempting to remove them from the computer.
8. After you have copied your files, exit Windows and shut down the computer.
9. Turn off the OPTO LCSX by turning off the yellow switch near the printer.
10. You have shut down the still. You may now leave the lab.

Ch.E. 327 Chemical Engineering Laboratory (Writing Enriched)

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ChE 327 Chemical Engineering Laboratory 1

General Information and Instructions

Objectives of the Course

1. To be able to use practical, problem solving methods based on use your

2. To be able to understand the capabilities and accuracy of many common methods

3. To be able to plan and execute experiments, which students will demonstrate by

4. To be able to successfully and cooperatively work with others, as demonstrated

5. To be able to analyze data, and write reports on time as demonstrated by the

Rev. 8/5/02 CRN, rev 7/31/10

5. Smoking, eating and drinking

6. Material Safety Data Sheets

7. General Safety and Waste

Rev. 8/11/02 rev 7/30/10

Schedules and Duties

Each experiment follows a schedule similar to the one outlined below:

Sample ChE Lab Schedule (your acutal schedule

Report Report Revised 2nd draft

Experiment 1 Experiment 2 Experiment 3

Duties of the Team Leader

2. Prepare the preliminary report.

4. Assign duties to individual team members.

5. Report any violation of laboratory policies and accidents to the lab

6. Ensure the general success of the laboratory experiment.

7. Attend all classes and meetings.

Duties of the Other Team Members

2. Perform duties assigned by the team leader.

4. Ensure the general success of the laboratory experiment.

5. Attend all classes and meetings.

6. Assist the team leader with the calculations.

Performance in lab 50%

Lab performance will be graded on leadership, understanding of the experiment, ability

Rev. 8/11/02 CRN

Data Acquisition and Control

Many of the laboratory experiments are interfaced to Opto22 SNAP LCSX

Opto22 Hardware - Basic Configuration with Computer Control:

1. Signal input/output (Analog I/O)

Up to 16 inputs or outputs can be handled by the boards in our systems.

Procedure for Using Factory Floor™ Software

1. Turn on computer, the and OPTO Board

Rev. 8/11/02 rev 7/30/10

Statistical Methods in Data Analysis

Ultimately experimental work results in a set of numbers that must be interpreted.

d) Multiple measurements involving three or more variables that are interrelated.

e) The planning of a set of experiments in a situation such as d) above so as to

A good example is given in Owen L. Davies, Statistical Methods in Research and

If we made a very large number of measurements, the envelope of the histogram

A common measure of the spread in the data is the STANDARD DEVIATION

These limiting quantities are used in expressing theoretical distributions.

Experimental data that fall on a NORMAL DISTRIBUTION curve are

Method of Least Squares

One frequently encountered problem in engineering is finding an equation to

Rev. 7/17/99, 8/11/02, 7/30/10

Mechanics and Form

Format, Pagination and Miscellaneous

9 Tables, Graphs and Charts

Drawings for Reports

In preparing your drawings of apparatus with its associated piping and

Occasionally it may be desirable to show a thermometer well or thermocouple

A differential pressure transmitter sending a signal to a computer or controller

JWH 11/17/86 rev. CRN 8/10/00 rev CRN 8/5/02

To determine the dynamic viscosity of a fluid using a Brookfield viscometer and a

1. Brookfield viscometer with small sample adapter, RV 21 spindle