ChE 135 HQRUV Laboratory Manual v2

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Chemical Engineering 135

Process Engineering Laboratory

Laboratory Manual

2017
Department of Chemical Engineering
University of the Philippines Diliman
Course Syllabus

A. ABOUT THE COURSE

Credit 2 units (6 hours lab)


Course
Descripti Experimental study of certain unit operations and processes.
on
Prerequis
ChE 133, ChE 134, ChE 125
ite

B. COURSE OUTCOMES

1. Design, Perform and evaluate experimental procedures on various unit operations and
processes
a. Explain rationale of procedure and equipment using the application of knowledge in
heat, mass and momentum transport, as well as chemical reaction engineering to
unit operations and processes
b. Make relevant observations, analyse sources of errors and modify procedures to
improve results
2. Interpret and draw conclusions from experimental results
a. Analyse data using relevant engineering approaches
b. Discuss and recognize engineering concepts as applied to the experimental results
3. Communicate, in a written and oral manner, clear and logical reports on experiments
and projects
4. Develop, execute and monitor collaborative investigative projects in process engineering
a. Create a feasible project plan according to specific objectives
b. Work as a team in a long-term project
c. Coordinate and collaborate with other teams in project implementation

C. Student Outcomes Satisfied by Course Outcomes


[a] Ability to apply knowledge of mathematics and science to solve engineering problems
[b] Ability to design and conduct experiments, as well as to analyse and interpret data
[e] Ability to identify, formulate, and solve engineering problems
[g] Ability to communicate effectively
[k] Ability to use the techniques, skills, and modern tools for engineering practice

D. GRADING SYSTEM

[92,100] [88,92) [84,88) [80,84) [76,80) [72,76) [68,72) [64,68) [60,64) [0,60
)
1.00 1.25 1.50 1.75 2.00 2.25 2.50 2.75 3.00 5.00

E. ASSESSMENT

CRITERIA PERCENTAGE
Experimental Design 10
Project Oral Report 10
Project Formal Report 5
Weekly Pre Laboratory
5
Report
Weekly Formal Report 60
Lab Performance 10
TOTAL 100

Full attendance in the Undergraduate Research Colloquium is required. Failure to meet this
requirement would result to a 10 point deduction in the final grade.

ChE 135 Laboratory Manual 1


Each student will have an initial 100 percent rating for the lab performance. Deductions shall
be given based on the Demerit System. A score below 60 will automatically result to a
grade of 5.

F. Schedule of Activities

Wee
Deliverables
k
Introduction and Syllabus Discussion
1 Jan 17 Jan 20
Assignment of Topics for Experimental Design
Attendance to Lab Use Orientation and Safety Seminar
2 Jan 24 Jan 27
Consultation for Experimental Design
3 Jan 31 Feb 3 Experiment 1
4 Feb 7 Feb 10 Experiment 2
5 Feb 14 Feb 17 Experiment 3
6 Feb 21 Feb 24 Experiment 4
7 Feb 28 Mar 3 Experiment 5
8 Mar 7 Mar 10 Experiment 6
9 Mar 14 Mar 17 Experiment 7
10 Mar 21 Mar 24 Experiment 8
11 Mar 28 Mar 31 Experiment 9
12 Apr 4 Apr 7 Experiment 10
13 Apr 11 Apr 14 Holy Week
14 Apr 18 Apr 21 Experimental Design Project Execution
15 Apr 25 Apr 28 Experimental Design Project Execution
16 May 2 May 5 Buffer Week
17 May 9 May 12 Project Oral Report

First draft of experimental design must be submitted on the day of your scheduled
consultation.
Final experimental design must be submitted by Week 3.
Project proponents are encouraged to begin preparations for the project as early as possible.

G. Experimental Design (ED)


1. The Experimental Design (ED) shall contain the following information:
Title
Give an appropriate title that will best describe the project as a whole
This will also be the title of the formal report

Introduction
Include relevant theory only aspects that would be cited/used in the project
Give some historical background in the context of the experiment (optional, if
applicable)
Use in-line citation for citing references. Use AMA (American Medical Association)
referencing format.
Statement of the Problem
General Objective
o State the objective of the entire project as a whole; give an overview of the
different tasks to be undertaken to achieve the general objective
o To be provided by the instructor
Specific Objectives
o State the objectives of each step to be done to achieve the general objective.
Include the parameters to be measured, assessed, or evaluated
Scope and Limitations
State the scope of the project (what tasks are to be done) and limitations (what
are not covered by the project)
State all assumptions to be made

ChE 135 Laboratory Manual 2


Methodology
Provide a step-by-step procedure. Adopt a numbered format for this section.
Risk Assessment
Identify the risks involved in the methodology. Follow laboratory form 3.
Guide Questions
Should contain questions addressed to the student, and serve as basis for the flow
of discussion in the Results and Discussion Reports
References
Properly cite all references used in the project proposal. Use AMA referencing
format.
Appendices
Include safety precautions (MSDS, if applicable) and waste disposal procedures (if
applicable)

H. PRE-LABORATORY REPORT
1. Each group is required to have one formal theme book sized pre-lab notebook.
2. Experimenters are required to accomplish a pre-lab before and after each experiment. It
should contain the following:
List of materials and chemicals needed (including the amount)
Schematic diagram of the procedure
Tables for data collection
3. All pre-labs must be submitted at least 2 working days before the scheduled date of the
experiment. No pre-lab on the day of the experiment, no experiment. A score of zero will be
given for the Formal Report of that experiment. Late pre-labs will receive a 15 point
deduction from the FR.
4. At the end of each experiment, all accomplished pre-lab must be submitted to the instructor
for checking. The experimenters must affix their signatures on every page of their pre-lab,
attesting that the reported data is correct.
Experimenters are discouraged from erasures as this would lower the credibility of the data.
If there are any erasures, have them countersigned by the instructor during the experiment
day.

I. FORMAL REPORT
Each group shall write a Formal Report (FR) after performing an experiment. The contents of the
FR are the following:

Abstract
The abstract must contain less than 200 words and should summarize the
methodology and results of the experiment.
Introduction
Provide a brief background on concepts involved and the rationale of the experiment.
Include relevant theory and historical context if applicable.
Materials and Methodology
This part must be in narrative form.
A schematic diagram of the set up should be included.
Results and Discussion
Present the computed results in the most meaningful form (e.g. graphs, figures,
tables).
Include computed uncertainties in the figures.
Use proper captioning in labelling figures, tables, etc.
Discuss your results in paragraph form.
Use in-line citation for citing references (APA).
Conclusions and Recommendations
Conclusions must have been explained in the Discussion section
Recommendations could be made with respect to experimental procedure, materials,
computational process, etc.
References
Properly cite all references used in the FR (APA).
At least three book/journal references must be provided. Ensure credibility of journal
article to be cited.

ChE 135 Laboratory Manual 3


Appendix: Sample Calculations
Show sample calculations performed on the raw data, including error propagation
No need to print out the raw data (it should be available in the logbook)

A printed copy and a soft copy of the FRs must be submitted before 7:30 am, a week
after the experiment was performed.
Late submissions shall be given a grade of zero, for whatever reason.
For each groups first experiment they will be required to combine their own results
with the results of the other groups for that same experiment and conduct further
statistical analysis using the multiple sets of data at the end of the experimental runs. This
formal report will be worth twice the weight of a regular formal report.

J. CLASS POLICIES

ChE 135 Logbook. An attendance logbook shall be provided for the course. Each page
must contain the experiment date, the instructors name, and the students present. All
students must log their time in and time out in the lab.
Tardiness. A student shall be marked late if he/she logged his/her name in the ChE 135
Logbook later than 8:00 AM (or an hour after the period starts). Two (2) late arrivals would be
counted as one (1) absence.
Absence. A student shall be marked absent if he/she has not logged his/her name in the
ChE 135 Logbook before 8:30 AM (or 2 hours after the period starts). A grade of 5.00 will be
given to a student with more than 3 absences (excused or unexcused).
Excused Absence. Excuses other than personal illness and bereavement are not valid. A
formal excuse letter, accompanied by a medical certificate and other documents if excuse is
due to personal illness, should be submitted within a week after the incurred absence.
Failure to comply with this requirement shall result to the nullification of the excuse.
Missed Experiment. A student who misses an experiment with a valid excuse will get a 5
point demerit in the Lab Performance and 60% of the group's grade for the Formal Report,
provided that his/her group mates vouch for his/her contribution. A student who missed an
experiment without a valid excuse will get a 10 point demerit in the Lab Performance and a
grade of zero for the FR.
Laptops. Use of laptops is prohibited on the experiment proper.
Group Participation. A group may opt to exclude certain member/s who do not contribute
to any course requirement. Consequently, excluded group member/s shall get a score of zero
for that requirement.
Starting an Experiment. The latest that an experiment may start is at 8 AM. Failure to do
so will result to demerits. At least two members of the group must be present to begin an
experiment. Once the experiment starts, the missing group members shall be considered
late.
University Rules on absences (max of 3)/cheating/dropping/LOA shall be strictly applied.
Academic dishonesty, in any form, will not be tolerated in this course and will be given a
grade of 5.
The instructor reserves the right to make changes in the class policies and schedules when
deemed necessary.

K. LAB PERFORMANCE

A student can get full credits for lab performance if he/she has complied with the following
requirements inside the ChE Laboratory at all times.

a. Personal Protective Equipment


Everyone is required to wear basic Personal Protective Equipment (PPE). This includes a
laboratory gown, safety goggles, closed shoes (semi-closed flats are not allowed), full-length
pants, face mask and rubber gloves. Slippers, sandals, shorts, skirts are not allowed.
Wearing of contact lenses is strictly prohibited. When handling hazardous chemicals, face

ChE 135 Laboratory Manual 4


masks and gloves are required. Students who fail to comply will not be allowed to perform
the experiment, and will thus be given a grade of zero for Lab Performance.

b. Procedure for Borrowing Materials

1. Write your Name in the MATERIALS section of the logbook, beside your experiment for
the day.
2. Claim Material Checklist and Material Basket from Laboratory Technician. Ensure that
the materials are complete and in good condition before proceeding.
3. Leave your ID with the Laboratory Technician.

c. Procedure for Returning Materials

1. Return Material Basket with Material Checklist to the Laboratory Technician. Inform
the technician if you broke or misplaced a material.
2. Laboratory Technician will check if the materials are complete and in good condition
using the Material Checklist from the student.
3. Claim your ID once checking is complete and deficiencies are recorded, if any.
4. To settle deficiencies, replace material and ask for a Proof of Settlement Form from
the Laboratory Technician to officially settle the deficiency.

d. Laboratory Guidelines
Work Procedure
Never work in the lab without supervision of an instructor.
Immediately report spills, accidents or injuries to the instructor.
Dont leave experiments in progress.
Make sure no flammable solvents are present in the vicinity when lighting a flame.
Do not leave any burners or hot plates unattended. Leave a note indicating the time the
burner or hot plate was last used after using. Do not place the note on top of the hot
burner.
Turn off all heating apparatus, gas valves, and water faucets not in use.
ALWAYS label glass wares with chemicals.
Do not remove equipment or chemicals from the laboratory.
Use equipment and glassware only for their intended use.
Notify teacher of any sensitivity to chemicals.
Do not use damaged glassware.
Do not use air compressors to dry glassware unless you know it contains water only.
Keep area free of water spills to avoid accidents.

Good Housekeeping
Food and drinks are not allowed inside the laboratory.
Never block exits, stairways and hallways.
Never pour chemical waste into sink drains or waste baskets.
Place chemical waste in appropriately labelled waste containers only.
Store bags and other personal items in designated area.
Keep floor clear of all objects (e.g. ice and spilled liquids) and keep your work area clean.
Never leave valuables unattended.

Emergency and First Aid


Know all exits, the location of the emergency phone, and the location of and how to
operate fire extinguishers, alarms, fire blankets, eye washes, first-aid kits, and
emergency showers.
In case of emergency or accident, follow the established emergency plan and evacuate
the building at the nearest exit.
Be familiar with common first aid procedures during incidents of burns, eye contact with
dust and chemical irritants, ingestion of chemicals, cuts and bruises from broken
glassware and machine parts.
Check first aid treatments and precautions from the MSDS of chemicals you will be
working with before an experiment.
Do not perform mouth-mouth resuscitation especially if toxic chemicals are involved.

ChE 135 Laboratory Manual 5


Lab Security
Secure exterior doors after normal operating hours.
Question the presence of unfamiliar individuals and report all suspicious activity to the
instructor.
Request for the use of lab facilities beyond office hours shall be pre-approved by the Lab
Manager.
Visitors are required to secure an ID pass.

e. Waste Disposal
A Waste Logbook for the course is provided. All chemical wastes should be disposed in
proper waste jars and logged in the logbook with the amounts indicated. If no waste jar is
available, request for one. If a waste jar is full, seek the lab instructor or the lab technician
for assistance. Do not fill the waste jar up to their maximum capacity.

L. DEMERIT SYSTEM

Demerit Minor Offenses


2 Not wearing of closed shoes
2 Not wearing safety glasses/goggles
2 Wearing of contact lenses
2 Excessively wet table top
2 Wet floor around the setup
2 Improper disposal of simple solids wastes (tissue, paper, masking tapes,
labels)
2 Not recording time in and time out in logbook
3 Not wearing of safety gloves for hot setups/when needed
3 Not wearing of rubber gloves for chemical setups/when needed
3 Improper cleaning (not removing label, not rinsed) and arrangement of
glassware
3 Playing with the thermocouple
3 Improper arrangement of bags and lab kits
3 Not returning of materials and equipment
3 Wearing of lab gown outside the pilot plant

Demerit Major Offenses


5 Use of unnecessary gadgets (except camera for documentation and
timer) for playing games, music, movies
5 Playing with the fire extinguisher
5 Improper chemical waste disposal
5 Improper disposal of broken glassware, returning of excess reagents to
the reagent bottle
5 Sleeping near the laboratory setup
5 Meddling with setups of other groups
5 Improper use of analytical balance
5 Spilling of reagents on or around the analytical balance
5 Experiment was started after 8AM
5 Beginning the experiment while unfamiliar with the procedure, MSDS,
and HSE considerations

Demerit Grave Offenses


10 Horse playing, unnecessary water spraying, playing of cooling water

ChE 135 Laboratory Manual 6


and ice
10 Eating and drinking inside the laboratory
10 Doing other requirements during experimental runs
10 Leaving a running laboratory setup
15 Permanent damage to an equipment or setup

M. LABORATORY CLEARANCE

The student is required to settle all broken or misplaced glassware, chemicals or equipment
indicated in the Clearance Section of the Materials Logbook. Failure to settle these deficiencies
can result to a grade of INC.

ChE 135 Laboratory Manual 7


EXPERIMENT NO. # 1

Kinetic Modeling of Glucose Fermentation by Bakers


Yeast
Introduction
Carbon dioxide may be produced from the respiration of Bakers yeast (Saccharomyces cerevesiae),
which is commonly referred to as fermentation. CO2 may be produced in two ways aerobic and
anaerobic depending on the presence of oxygen. Shown below are the balanced reactions:

Anaerobic reaction: C6 H 12 O6 2 C 2 H 5 OH +2 C O2+ 2 ATP


Aerobic reaction: C6 H 12 O6 +6 O2 6 C O2 +6 H 2 O+ (1618 ) ATP

Before upscale of a unit process from reactants to products, one must know the kinetics of a reaction by
modelling the rate of a reaction or the concentration of the reactants or products through time. The
kinetics of a chemical reaction can be analyzed by different methods, such as (1) method of initial
rates, (2) fractional-life methods, (3) integral analysis and (4) differential analysis. In this experiment
we will study the rates of an enzymatic reaction using methods (3) and (4).

Objectives, Scope and Limitations


(1) Determine the kinetic model of the enzymatic reaction through glucose fermentation.
(2) Determine the effect of concentration and temperature* on the rate of glucose fermentation.
(3) Determine whether the fermentation is aerobic or anaerobic.
(4) Determine the kinetic parameters using integral and differential analysis.

Scope and Limitations:

The experiment is limited on the effects of glucose concentration only and not yeast
concentration.
Temperature effects will only be discussed by the main group assigned to this experiment.
The experiment is limited on the modelling of kinetic data and calculation of kinetic
parameters. It does not involve formulation of a reaction mechanism using elementary
reactions.

Methodology
A. Materials and Apparatus

Equipment Materials Reagents


Analytical balance (1) 500 mL Buchner flask Bakers yeast
Thermometer (1) 50 mL burette Anhydrous glucose
Hot plate with magnetic 0.400 M acetic acid-
(1) 50 mL beaker
stirrer acetate buffer
Batch reactor setup (3) 250 mL beakers Distilled water
Metal pan Watch glass Tap water
Graduated cylinder
Stopwatch
Spatula
Stirring rod
Metal clip
Iron clamp
B. Procedure
1. Assembling the setup
a. Assemble the setup as shown by Figure 1.
b. Fill basin with tap water. Invert the burette into the basin.

ChE 135 Laboratory Manual 1


c. Secure the burette by using an iron clamp. Make sure the burette is not slanted. It
must be perpendicular to the basin or water level.
d. Attach rubber tubing into the Buchner flask and into the inverted burette.
e. Use an aspirator to adjust the water level to 50 mL. To check for gas leaks, make sure
that the water level does not decrease while the metal clip is secured.

Figure 1. Fermentation setup.

2. Solution preparation
a. Prepare the assigned glucose solution. The sugar solution must be sufficient for three
trials. Set aside.
Assigned glucose solutions:

Groups 1,4,7 2,5,8 3,6,9


Glucose solution 0.125 0.250 0.500
concentration (%w/v)

b. Prepare 1% w/v yeast solution. Dissolve sufficient yeast powder to distilled water
heated to 50 C. Set aside and allow 20-30 minutes for the yeast cells to re-suspend.
*Note that the concentrations are in %w/v of the whole reaction mixture (50mL)
3. Measuring the reaction rate
a. Preheat the water bath to 30C.
b. Place the glucose solution on the water bath. Preheat the glucose solution to the
assigned temperature.
c. Pour 12.5 mL of the yeast solution and 12.5 mL of the buffer solution into the Buchner
flask. Place the Buchner flask on the water bath. Heat this mixture to 30C. Place the
magnetic stirrer inside the Buchner flask and the set the magnetic stirrer speed to
500 rpm.
d. Quickly combine 25 mL of glucose solution with the yeast and buffer solutions in a
Buchner flask.
e. Quickly cover the Buchner flask with a rubber stopper then set the magnetic stirrer
speed to 1500 rpm.
f. Record the initial volume after loosening the metal clip. Note that the initial
volume is not 50 mL but the volume after loosening the metal clip.
g. Record the volume of the water inside the burette every 30 seconds until no
significant change in the volume is observed after three successive readings, until all
of the water in the burette is displaced or until 1 hour. In case all of the water has
been displaced, record the time this happens.
h. Do steps (a)-(g) for three replicates.

Notes
1. Applying too much pressure in connecting the rubber tubing might cause glass breakage.
2. Use thicker rubber tubing if there are gas leaks.
3. Be careful using the aspirator in adjusting the water level. If the water level exceeds the
inverted burette the water might go through inside the aspirator.
4. No water should flow into the section of the tubing blocked by the metal clip. Make sure the flow
inside the tube is not blocked by bends or folds.
5. Know the center of the stirrer before allowing the stirrer to spin.

ChE 135 Laboratory Manual 2


6. The experimenter recording the time and the experimenter reading the water level must be the
same throughout the study.

Guide Questions
1. Based from the kinetic data, is the reaction aerobic or anaerobic?
2. What is the effect of concentration to the rate of glucose fermentation? How does your kinetic
data tell the nature of enzymatic reactions?
3. How do you interpret your kinetic data using integral analysis? Show your derivations and your
calculated parameters.
4. How do you interpret your kinetic data using differential analysis? Show your derivations and
your calculated parameters. Discuss the advantages and disadvantages between integral and
differential analysis.
5. There are three known linearized Michaelis-Menten plots for differential analysis. Calculate the
kinetic parameters for each plot and give their advantages and disadvantages.
6. What measures were undertaken to ensure that the reaction is only affected by the sugar and
yeast concentration? Were these necessary?

References
Chemical Engineering 135: Process Engineering Laboratory Manual (2015). Department of Chemical
Engineering, UP Diliman.

Atkins, P. W. (2014). Atkins' Physical Chemistry. Oxford: Oxford Univ. Press.

ChE 135 Laboratory Manual 3


Group Members: _________________________________________ Date &Time
Started:________________
_________________________________________ Date &Time Finished:_______________
_________________________________________ Noted: __________________________
_________________________________________

Kinetics of Glucose Fermentation

________________________________________________________________________________________________

Sugar concentration (%w/v)


Yeast Concentration (%w/v)
%w/v of reagent in reaction mixture

Summary of Replicates

Replicate #1

Initial volume of water in burette (mL)


Final Volume of water in burette (mL)
Total time of reaction (min)

Replicate #2

Initial volume of water in burette (mL)


Final Volume of water in burette (mL)
Total time of reaction (min)

Replicate #3

Initial volume of water in burette (mL)


Final Volume of water in burette (mL)
Total time of reaction (min)

Replicate #1 Replicate #2 Replicate #3


Volume of Volume of Volume of
Time (min) water in Time (min) water in Time (min) water in
burette (mL) burette (mL) burette (mL)

ChE 135 Laboratory Manual 4


EXPERIMENT NO. 2

ChE 135 Laboratory Manual 5


GENERATING OPERATING CURVES FOR VARIOUS PUMP
OPERATION
Introduction
Pumps are devices used to help move fluids from one point to another through mechanical work. Pumps
transfer energy to the fluid, increasing its velocity and/or pressure, which in turn, helps the fluid
overcome physical barriers such as friction and height difference. There are two main types of pumps:
Positive displacement and Kinetic or Dynamic Pumps. An example of a kinetic pump is a centrifugal
pump.

Centrifugal pumps operate by converting kinetic energy to pressure. A weir will be used to measure the
flowrate of the discharge from the pump(s). The change in height h (m) in the stilling well can be
related to the flowrate Q (m3/s) using the empirical formula

8
Q= 2 g C e (h+0.00085)5/ 2
15

where g is the acceleration due to gravity and Ce = 0.5765. The suction pipe and the delivery pipe
diameters are known to be 31.75 mm and 25.4 mm, respectively.

Fig 2. Schematic Diagram of the Pump Test Rig

Objectives, Scope and Limitations


The experiment will utilize a pump test rig with two centrifugal pumps. It will focus on the energy
balance around the pumps. The friction losses will be lumped with the total head. Since the pressure
gauge for the suction of pump 2 is not functional, the suction head for pump 2 will be assumed zero.
The experiment requires the application of concepts from fluid mechanics. At the end of the
experiment, students are expected to:

1.Know how to operate the pump test rig


2.Understand how the valves are used to attain the desired pump operation

ChE 135 Laboratory Manual 6


3.Take the relevant readings from the pressure gauges and the stilling well
4.Perform the energy balances, taking into account reasonable simplifying assumptions
5.Generate a plot of the total head versus flow rate for each of the pump operations (single, series, and
parallel)

Methodology

A. Materials and Apparatus

1 Series/Parallel Pump Test Rig

B. Procedure
1. Preliminary step: Preparing the setup
a. Ensure that the valves are closed.
b. Fill the approach channel up to the apex of the V-notch with water. Ensure that the suction pipes are
submerged in water, and will remain so during operation.
c. Adjust the hook in the stilling well until it touches the water level. Set the point gauge to zero.
d. Open all the valves, except for the flow regulating valve, and turn the motor on.
e. Gradually increase the speed to 2000 rpm. Open the flow regulating valve.
f. Close the flow regulating valve, gradually set the speed to zero, and turn off the motor.
2. Data gathering
a. Adjust the valves to obtain the desired pump operation. Keep the flow control valve closed.
b. Turn the motor on. Note the reading on the relevant pressure gauges.
c. Gradually increase the speed to 2000 rpm. Note the relevant pressure gauge readings.
d. Open the flow control valve by approximately one turn (360 degrees). Wait for the water level in the
stilling well to become steady.
e. Note the relevant pressure gauge readings and the water level in the stilling well.
f. Repeat steps d and e until the flow control valve has been opened by 10 turns.
g. Close the flow control valve. Gradually set the speed controller back to zero. Close the other valves.
Turn the motor off.

Notes
1. The pressure gauge for suction of pump 2 is not functional.
2. Make sure that the suction pumps are submerged during operation.
3. The pump connections might slightly leak.
4. Point gauge must be calibrated.

Guide Questions
1. How does each of the valves affect water flow in the setup? What adjustments can be made to direct
the water and achieve the desired operation?
2. What trend(s) can be observed from the pump operating curves?
3. What differentiates series from parallel pump operation? How do the respective operating curves reflect
this difference?

References
Armfield Limited. Series/Parallel Pump Test Rig Instructional Manual. Issue 4.
Green D, Perry R. Pumps and Compressors. In: Perry's Chemical Engineers' Handbook. 8th ed.; 2008.

ChE 135 Laboratory Manual 7


Group Members: _________________________________________ Date & Time
Started:________________
_________________________________________ Date & Time Finished:_______________
_________________________________________ Noted: __________________________
_________________________________________

Pump Curve Generation

Pump 1

No. of turns Height in the stilling well, Suction Head, m Discharge Head, m Q,m3/s
mm

10

Pump 2

No. of turns Height in the stilling well, Suction Head, m Discharge Head, m Q,m3/s
mm

ChE 135 Laboratory Manual 8


10

Series

No. of turns Height in the stilling well, Suction Head, m Discharge Head, m Q, m3/s
mm

10

Parallel

No. of Height in the stilling Suction Head Discharge Head Discharge Head Q, m3/s
turns well, mm 1, m 1, m 2, m

10

ChE 135 Laboratory Manual 9


ChE 135 Laboratory Manual 10
EXPERIMENT NO. # 3

DETERMINATION OF SCREEN EFFECTIVENESS

Introduction
Mechanical separations are based on physical differences between the particles such as sizes and
shapes. One of the general method for mechanical separation is the use of screens. It is a method for
separating based on the size of the particles only. A single screen can separate particles into two
fractions. The particles that pass through the screen are called undersize. The particles that did not
pass through are called oversize. Screening is more commonly done dry or with low moisture content.

To determine the success of screens in separating the materials, the effectiveness of the screen must
be calculated. For a completely effective screen with a feed composed of materials A and B, all portions
of the material A would be in the overflow and material B would be in the underflow. The product of the
screen effectiveness of the undersize and oversize material will determine the combined overall
effectiveness as shown below.

D x D B ( 1x B )
effectiveness=
F xF F ( 1x F )

Where F is the feed flow rate, D is the overflow flow rate, B is the underflow flow rate and x i is the mass
fraction of the corresponding flow rate.

Objectives, Scope and Limitations


General Objectives:
To design an experiment that will demonstrate the applications of previous chemical engineering
courses
Specific Objectives:
To do a size distribution analysis of sand using a certain set of sieves
To determine the effectiveness of 4-mesh and 20-mesh screens

Scope and Limitations:


This experiment focuses only on sand as the feed for the screening process. The experiment is done to
determine the size distribution of sand in a specific set of sieves (4, 8, 12, 16, 20, 50,70,100,140-
mesh). Only screens with mesh size of 20 and 100 are used since these are the only screens with
corresponding sieves in the laboratory. It is assumed that the sieves are effective. The experiment does
not take into account the inefficiencies of the sieves for the size distribution analysis. Other factors
such as impurities in sand, randomness of the particle sizes of the sand, and blinding in the screens and
sieves are also not considered in the experiment.

Methodology
A. Materials and Apparatus

Materials: Apparatus:
Sand Analytical Balance
Pan Vibrating Screen
Shaker
Screens (20,100-mesh)
Sieves (4, 8, 12, 16, 20, 50,70,100,140-
mesh)

B. Procedure

ChE 135 Laboratory Manual 11


Part I: Particle Size Distribution of Sand
1. Measure the weight of the all sieves (mesh size 4, 8, 12, 16, 20, 50, 70, 100 and 140) and the
catching pan to be used.
2. Weigh 1500g of sand.
3. Pour the sand onto the topmost sieve, and place the catching pan on the bottom of the pile.
Cover the topmost sieve.
4. Place the sieves to be on the sieve shaker. Clamp the topmost sieve tightly, and further secure
the clamp with a c- clamp.
5. Operate the sieve shaker for ten minutes. In order to prevent the shaker from moving, apply a
weight on the wooden supports.
6. Measure the weight of each combined sieve and sand. Record the combined weight. Set aside
the sand used for Part II., and make sure to minimize material loss.
7. Obtain the particle size distribution. Calculate the average diameter of the sand.

Part II: Determination of Effectiveness of the Screening Set-Up


1. Measure the weight of the pan.
2. Place the mesh 20 screen at the top and the mesh 140 screen at the bottom of the mechanical
shaker set-up.
3. Pour the sand from Part I onto the topmost screen.
4. Turn on the mechanical shaker and wait for two minutes. Make sure to maintain at least a
distance of at least two feet from the mechanical shaker, unless your weight is used as an
additional support to prevent the shaker from moving.
5. Pour the contents of the first screen onto a collecting pan and weigh the combined weight.
Record the resulting weight.
6. Do a sieve analysis as in Part I 3-6 for the contents of the 1st screen.
7. Repeats steps 5-6 for the mesh 100 screen and the catching pan.

Repeat Parts I and II for a further two trials.

Notes
1. Vibrating screen operates at 110 V.
2. Shaker operates at 110 V.
3. Vibrating screen operates violently, do not leave it while it is running.
4. Properly secure sieves into shaker. Fasten a clamp after securing the sieves.
5. Do not leave the shaker while it is running.

Guide Questions
1. What is the importance of weighing each sieve before and after sieving?
2. Is the obtained weight from screening matches the original weight (1500 g)? If not, what are the
sources of error?

References
McCabe, W., Smith, J., &Harriott, P. (1993). Unit operations of chemical engineering. New York: McGraw-
Hill.

ChE 135 Laboratory Manual 12


Group Members: _________________________________________ Date &Time
Started:________________
_________________________________________ Date &Time Finished:_______________
_________________________________________ Noted: __________________________
_________________________________________

Determination of Screen Effectiveness

TRIAL # __

Part I.
Initial Weight of Sand: __________
Table I.
Sieve Mass of sieve Combined mass of sieve and sand Mass of sand in sieve
Mass fraction
Number (g) (g) (g)

12

16

20

50

70

100

140

Bottom Pan

ChE 135 Laboratory Manual 13


Part II.
Table II
Combined mass of sand and collecting pan (g) Mass of sand (g)
Screen # 20
Screen # 100
Catching Pan

Mass of collecting pan: _______

Table III A: Mesh 20 Screen

Sieve Number Combined mass of sieve and sand (g) Mass of sand in sieve (g) Mass fraction

12

16

20

50

70

100

140

Bottom Pan

ChE 135 Laboratory Manual 14


Table III B: Mesh 100 Screen

Sieve Number Combined mass of sieve and sand (g) Mass of sand in sieve (g) Mass fraction

12

16

20

50

70

100

140

Bottom Pan

Table III C: Catching pan

Sieve Number Combined mass of sieve and sand (g) Mass of sand in sieve (g) Mass fraction

12

16

20

50

70

100

140

Bottom Pan

ChE 135 Laboratory Manual 15


EXPERIMENT NO. 4

DETERMINATION OF SETTLING CHARACTERISTICS OF


KAOLIN POWDER USING BATCH SETTLING TESTS
Introduction
Sedimentation is a solid-fluid separation process. In this process, a dilute slurry separates into a clear
fluid and a slurry of higher solids content under the influence of gravity.

Batch sedimentation is performed to characterize the sedimentation behavior of slurry. In this


experiment, the effect of several factors on the sedimentation behavior of Kaolin Powder-Water slurry
will be investigated.

Objectives, Scope and Limitations


Determine the effect of slurry concentration on the settling behavior of kaolin.
Generate a plot of height vs. time for different slurry concentrations.

Methodology
A Materials and Apparatus

Equipment: Reagents: Apparatus:


Sedimentation set-up Kaolin powder One (1) 1 L beaker
Platform balance Tap water One (1) 250 mL beaker
One (1) 1 L graduated
cylinder
Spatula/scooper
Stirring rod
B Procedure
1 In this experiment you will be preparing the following solutions:
Table 3. Slurry concentrations

Slurry Concentration (%w/v)


Group 1,4,7 2,5,8 3,6,9
Tube A 2.0 3.0 4.0
Tube B 6.0 7.0 8.0
Tube C 2.0 3.0 4.0

Tube C also contains 0.1%w/v of alum.


2 The sedimentation tube has a 2L capacity. Measure the amount of kaolin, and water
necessary to prepare solutions in 1.
3 Prepare the solutions in bulk as much as possible.
4 Transfer the prepared solutions to the sedimentation tubes. The tubes must be at least 90%
full.
5 Record the height of the settling zones for the three tubes.

Notes
1 Be very cautious with handling large glass equipment.
2 Avoid inhalation and contact of kaolin with eyes. Use a mask and a pair of gloves when handling
kaolin. (weighing, solution preparation)
3 Kaolin powder tends to form lumps during solution preparation. Make sure that the solutions are
well mixed before start of observation.
4 Start observing and measuring the 3 tubes at the same time.

Guide Questions
1 What settling zones are evident in the system?
2 What properties of the slurry could be derived from the data?
3 How did initial concentration affect the sedimentation behaviour?

ChE 135 Laboratory Manual 16


Alternatives
The following experimental design can be used to observe the effect of coagulants.

Table 4. Alternative experimental design.

Tube Slurry Composition Coagulant


A 2.5 wt% kaolin ---
B 3.5 wt% kaolin ---
C 2.5 wt% kaolin 0.1 wt% alum

References
Mardles, E. W. J. Viscosity and Sedimentation of Kaolin and Bentonite in Organic Liquids. Clay Minerals
0.2 (1948): 41-43. PDF.

ChE 135 Laboratory Manual 17


Group Members: ____________________________________ Date &Time
Started:________________
____________________________________ Date &Time Finished:_______________
____________________________________ Noted: __________________________
____________________________________

Settling Characteristics of Kaolin Powder


Time Tube A Tube B Tube C

ChE 135 Laboratory Manual 18


EXPERIMENT NO. 5

UNSTEADY FLOW: DRAINING OF A TANK


Introduction
In fluid mechanics, fluid flow may be classified as steady or unsteady. Unsteady flow is a general term
used for those that have properties, velocity, temperature, etc., changing with time. The term transient
is usually interchanged with unsteady but it is typically used in developing flow. The term periodic, on
the other hand, refers to an unsteady flow that oscillates about a steady mean (Cengel & Cimbala,
2014).

One of the applications of unsteady flow is the draining of water from a reservoir in which the head is
varying with time. It could be used to estimate the summation of loss coefficients of the system. Using
a cylindrical reservoir, and under the assumptions of isothermal, incompressible flow and negligible
skin friction, the overall mechanical energy balance could be simplified to the following equation:

a
A 2 ( 1+ K )
g
( ho h )=t

where
A = cross-sectional area of the reservoir
a = cross-sectional area of the pipe
g = acceleration due to gravity
ho = initial height of the water in the reservoir
h = height of water at time t
t = time in seconds
K = summation of loss coefficients

The equation above can then be used to plot the height of the water versus time in order to obtain the
parameters needed.

Objectives, Scope and Limitations


The objectives of this experiment are to determine and verify the relationship between height and time
with regards to the draining of a tank filled with water; to estimate the friction losses within a tank
system by using the mechanical energy balance equation and continuity equation, and; to compare
experimentally determined values of the loss coefficient with reported literature values. On the other
hand, the coverage of this experiment is limited only to quasi-steady flow, a subset of unsteady flow
characterized by the absence of inertial or elastic effects on flow behavior; consequently, other types of
unsteady flow (e.g. rigid column flow, water hammer) will not be treated. The container composed of
plastic shall thus be assumed perfectly rigid and non-deformable.

Methodology
A. Materials and Apparatus

Reagents Materials Apparatus


Water Ruler/measuring tape Cylindrical tank with
Time-measuring attached ball valve
instrument (stopwatch,
camera, etc.)

B. Procedure
1. Measure the diameter of the tank and the diameter of the pipe. Record these values as D t
and Dp, respectively.
2. Close the ball valve completely. Fill the container with water until a height h o of 80 cm is
measured from the discharge level to the water surface.

ChE 135 Laboratory Manual 19


3. Open the ball valve completely. Record the variation of height with time with either a
stopwatch or a camera. Six to ten data points of height versus time are recommended for
analysis.
4. Repeat steps 2-3 with the same initial height for a total of three trials.
5. Repeat steps 2-4 for ho = 60 cm and ho = 40 cm instead.

Experiment Set-up

Figure 3. Cylindrical tank with attached ball valve

Notes
1. Handle the set-up carefully and work near the sink.
2. Keep in mind that the draining may be too fast to record data.
3. Ensure that the valve is fully opened throughout the recording of data. Otherwise, the
inconsistency of valve opening may lead to significant error in computed values.
4. Always keep the top end of the tank open during the experiment. Else, expect to get wet
accompanied by an implosion.
5. Make sure that the tank is supported by another person upon opening the valve to prevent any
spills.

Guide Questions
1. What is the effect of decreasing initial height of the water to the draining time?
2. Do the results of the experiment follow the assumption that the system is frictionless? Compute

for the theoretical K , not accounting skin friction. Is there a difference between the

theoretical and experimental K values?

3. What is the relationship of the initial height of the water to the value of K ? What could be
the reason for such trend?
4. Is the gravitational constant determined from the Bernoulli equation similar to/different from the
literature value? Is there a trend in the values of the computed gravitational constant for
different initial heights?
5. What could be the sources of error?

Alternatives
An alternative setup with an additional flow metering capability can also be used to evaluate the
unsteady flow behaviour of a draining tank. The setup used is shown in figure 5.

ChE 135 Laboratory Manual 20


Figure 4. Cylindrical tank with attached ball valve

The alternative procedure is as follows:

1. Measure the radii of the orifice and the tubing in the experimental set-up provided. Ensure
that water will not leak anywhere in the setup.
2. Turn on the water supply. Allow the system to reach steady state by controlling the water
flow into the tank.
3. Once the system has reached steady state, use a beaker to catch the water leaving the tank.
Start the timer at the instant when the stream enters the beaker, and stop the timer when
100 mL of the water has been collected. At the same time, measure the height difference of
the water levels in the improvised manometer.
4. From the resulting data, compute for the cross-sectional area of the orifice, volumetric flow
rate, and the pressure before and after the orifice. Solve for the orifice constant from these
values.
5. Fill the tank with water until it is nearly full. Block the flow of water with a finger before
unloading the tank.
6. Position a beaker where the water is expected to land. Tape a ruler parallel to the tank for
liquid height measurements; the zero line of the ruler should be positioned at the level of the
horizontal tubing.
7. Place a camera such that the water jet and the ruler can be captured sideways.
8. Unblock the water flow and start the timer. Record the height of the water inside the tank
every 10 seconds until the tank is about halfway drained. At this instant, stop the timer and
the camera recording.
9. Use ImageJ to measure the vertical and horizontal distances travelled by the water jet for
each 10-second measurement. From these data, use the concept of projectile motion to
compute for the velocity of the water jet.
10. For the determination of relationship between water height and pressure drop, repeat steps
6 to 9, but measure the height differences inside the manometer as well.

References
Cengel, Y. A., & Cimbala, J. M. (2014). Fluid Mechanics: Fundamentals and Applications Third Edition.
New York: McGraw-Hill.

ChE 135 Laboratory Manual 21


Group Members: _________________________________________ Date & Time
Started:________________
_________________________________________ Date & Time Finished:_______________
_________________________________________ Noted: __________________________
_________________________________________

Unsteady Flow
____________________________________________________________________________________
Diameter of tank, Dt (m)
Diameter of pipe, Dp (m)

ho =0.8 m

Trial 1 Trial 2 Trial 3


h (m) t (s) h (m) t (s) h (m) t (s)

ho =0.6 m

Trial 1 Trial 2 Trial 3


h (m) t (s) h (m) t (s) h (m) t (s)

ho =0.4 m

Trial 1 Trial 2 Trial 3


h (m) t (s) h (m) t (s) h (m) t (s)

ChE 135 Laboratory Manual 22


EXPERIMENT NO. # 6
Unsteady Heating of Water in Flow Systems
Introduction
Heat transfer is the exchange of thermal energy between physical systems by means of the
temperature difference between them. This transfer may well occur steadily or unsteadily. Under
steady state conditions the temperature within the system is invariant with time. On the other hand,
the temperature within the system does vary with time under unsteady state conditions.

In practice, no system exists immediately under steady state conditions. Unsteady state conditions are
always a precursor to steady state conditions. After heat transfer is initiated, time must pass before the
system becomes steady. During this period of transition the system is behaves unsteadily.

No system can likewise remain under unsteady state conditions. The temperature of the system will
eventually reach the temperature of the heat source, and once this happens, the system will be at
steady state. Even if the amount of heat being transferred into the system is increased, the system at
some point will reach its critical temperature. The energy flowing into instead causes phase changes
within the system rather than an increase in temperature.

Objectives, Scope and Limitations


This experiment aims to:
Demonstrate unsteady heating for a flowing water system
Be able to apply overall energy and mechanical energy balances in order to characterize the
system.
Be able to determine using the setup the mean heat capacity (Cp) of water in ambient
conditions

Be able to observe and determine when thermal equilibrium is reached in the system.

In this experiment, it is assumed that no heat and friction losses, the heat capacity and density of water
are constant, the flow rate and the control volume of the system are constant.

Methodology
A. Materials and Apparatus

Quantity Materials
2 Styrofoam Box (1 with weir and spout)
1 Water Heater
1 Thermocouple
1 Thermometer
1 rubber tube
1 Rubber Aspirator
At least 2 Buckets or Basins

B. Procedure
a. Batch Heating
1. Place an amount of water in a Styrofoam box enough to completely
submerge the water heater. Measure its weight and initial temperature.
2. Submerge the water heater into the setup and plug the water heater to
start heating. Ensure constant agitation of the water to avoid the lag of the
thermocouple in measuring the temperature.
3. Measure the temperature of the water in time intervals. Preferably, limit
the temperature to just before boiling.
4. Repeat steps 1-3 for a second trial.

b. Continuous Flow and Heating


i. Setup

ChE 135 Laboratory Manual 23


1. Place the Styrofoam box (without weir), Box 1, in the sink and fill it with
water.
2. Place the other Styrofoam box (with weir and spout), Box 2, at a lower
level to establish a considerable amount of elevation head. The elevation head
shall be set-up according to the table below:
Table 5. Experimental design.

Group Number 1 2 3 4 5 6 7

Height from top of Box 1 to top of Box 2 for 3 6 9 12 15 18 21


Trial 1(in)

Height from top of Box 1 to top of Box 2 for 12 15 18 21 3 6 9


Trial 2 (in)

3. Create a siphon using the rubber tube and connect Box 1 to Box 2. To start
the siphon, use an aspirator to create initial suction.
4. Place the water heater and the end of the siphon at distance farthest from
the weir.
5. To ensure a constant height difference, let the water in box 1 overflow
while continuously supplying it with water from the faucet. Before heating, wait
until both the Styrofoam boxes are full. You may opt to place a clamp on the spout
of box 2 to be able to control the flow and allow for faster filling.
6. Measure the height difference from the top of Box 1 and the spout at Box
2. Also, measure the inner diameter or the orifice of the spout attached to Box 2.
Record these values for each trial. Verify and record the size of the control volume
by measuring the height, width and length of the rectangular prism bounded by
the weir in Box 2 before the orifice or spout.

ChE 135 Laboratory Manual 24


ii. Heating
1. Place the thermocouple in Box 2 where the water goes after overflowing
from the weir. Use a bucket or a basin to collect the water coming from Box 2. Be
sure to determine the dry weight of the bucket or basin before using it.
2. Measure the temperature of the water in Box 1 using a thermometer, and
then a thermocouple. Note any discrepancies or differences in the given
temperatures.
3. Start heating. A weir induces natural convection currents in the cell where
the water is being heated, forcing even temperature distribution in the water
leaving the cell through the weir.
4. Record temperature reading after every 20 seconds, recording the exact
time using a split timer. Weigh the bucket or basin every after 2 minutes and
empty it for the next batch of weighing. Record the weight of water. Do these until
the temperature reading is constant for three consecutive observations.
5. Upon finishing heating, disconnect the heater from the power outlet.
Dispose of all remaining water to the sink. Repeat the set-up and heating for
another trial.

Figure 5. Experimental Setup

Notes

1. The electric water heater may give off electrical current, causing shock. As a precaution, it is
advised to do the following:
a. Do not touch the water while the water is being heated.
b. Ensure that closed, rubber-soled and dry footwear is worn.
c. Check the electric water heater and its wires for damage or exposed elements. Do not
use equipment with damaged wiring.
d. When in doubt, disconnect the electric heater from the power outlet.
2. Weigh all fluids by difference. This means that the container is first weighed dry, and its weight
recorded. The fluid and container are then weighed together and the weight of the fluid is found
by subtracting dry weight from the combined weight of the fluid and container.
3. It is considered best practice to lid of the boxes while the experiment is on-going. This is to
minimize heat loss.
4. Ensure that buckets and/or basins are in place to catch the water before any siphon is run. This
is to minimize spills on the laboratory floor.
5. It is best to place the lower end of the siphon beside the water heater.

Guide Questions
1. Using a mechanical energy balance, does the calculated flow rate of water is consistent with the
measured flow rate via pail method? Explain the differences, if any and state how it may affect
the overall energy balance of the system.

ChE 135 Laboratory Manual 25


2. How does changing the head vary the steady-state temperature reached by the system? How is
the unsteady-state behavior of the system affected by variations in head (i.e., does the time it
takes to reach steady state change)? Discuss why the behavior changes are observed.
3. Discuss why the batch set-up was manually agitated while the flow set-up was not. How does
the presence or absence of flow affect the mixing for each set-up?
4. From the general energy balance, derive an unsteady state energy balance equation that relates
T with respect to time. Make necessary assumptions and discuss its validity.
5. How is convection currents reflected in the unsteady-state energy balance derived? If not, why is
this so?

References
Hagen, K. (1999). Heat transfer with applications. Upper Saddle River, N.J.: Prentice Hall.

ChE 135 Laboratory Manual 26


Group Members: _________________________________________ Date &Time
Started:________________
_________________________________________ Date &Time Finished:_______________
_________________________________________ Noted: __________________________
_________________________________________

Unsteady Heating

Table 1. Batch Heating


Trial 1 Trial 2
Time ( ) Temperature ( ) Time ( ) Temperature ( )

Table 2. Continuous Flow & Heating (Trial 1)


Time ( Temperature ( mwater ( ) Time ( Temperature ( mwater ( )
) ) ) )

Elevatio
n:

ChE 135 Laboratory Manual 27


Table 3. Continuous Flow & Heating (Trial 2)
Time ( Temperature ( mwater ( ) Time ( Temperature ( mwater ( )
) ) ) )

Elevati
on:

ChE 135 Laboratory Manual 28


EXPERIMENT NO. # 7

DETERMINATION OF THE VISCOSITY OF SUGAR


SOLUTIONS
Introduction
Viscosity is a measure of a fluids resistance to flow or more specifically to gradual deformation by
shear stress or tensile stress. Viscometers are instruments used to measure the viscosity and flow
parameters of fluids. Viscometers used today are based on three phenomena which are a moving
surface in contact with a fluid, an object moving through a fluid, and fluid flowing through a resistive
component. The second phenomenon will be the focus of this experiment as it will exhibit the
mechanism of a falling ball viscometer. This method is normally used to measure the viscosity of
Newtonian liquids and gases. The experiment will be an application of Newtons law of motion
considering a force balance on a falling spherical ball when it reaches terminal velocity.

Objectives, Scope and Limitations


This experiment aims to determine the viscosity of the prepared sugar solutions using the measured
falling length and the time elapsed passing this length, and to determine the relationship between the
concentration and the calculated viscosity of the prepared sugar solutions.

In this experiment, the fluids that will be used are sugar solutions with concentrations of 10%, 20%,
30%, 40%, 50% and 60% by weight using refined white sugar.

Methodology
A. Materials and Apparatus

4 mm glass beads Burette


Refined white sugar Hot Plate

B. Procedure
Preparation of Sugar Solutions
1. In a large beaker, mix 300 grams of refined white sugar with 200 mL of water. Stir constantly
over a hot plate until no sugar crystals are visible. This will serve as the stock solution with
60% by weight concentration to be used to prepare the other solutions.
2. Load the graduated cylinder on the analytical balance and tare. Calculate the required mass
of stock solution to be transferred to the graduated cylinder using the dilution equation of
mass and weight fraction: M1 = x2M2/x1 where x2 and M2 are given in Table 1 and x1 is always
0.6. As a quick check, M1 should always be less than M2.
3. Once the required mass of stock solution is transferred to the graduated cylinder, dilute this
solution until the analytical balance reads M2. That is, add enough water until M1 reaches M2.
4. Measure the density of each solution, record in Table 1.
5. Set aside until all solutions reach room temperature.

Determination of Viscosity
1. Apply permanent marker to the 4mm glass bead. Measure its mass and record in Table 1.
2. Mark two convenient points in the burette, label the higher as point A and the lower as point
B. Preferably, choose the top end of the burette and the start of the funnel-shaped
contraction near the bottom end.
3. Measure the distance between these two points. Record in Table 1.
4. Fill the burette with the appropriate sugar solution with reference to Table 2 such that both
points are covered.
5. Drop the glass bead into the burette. Measure the time it takes for the glass bead to travel
from point A to B.
6. Record in Table 2. Repeat six trials per solution.

ChE 135 Laboratory Manual 29


Fig 6. Experimental Setup on Determination of Viscosity

Guide Questions
1. What properties of the sugar solution change in varying concentration?
2. How does the variation in concentration affect the movement of the glass bead?
3. Suggest a model that relates the concentration with the viscosity of any sugar solution.
4. Can Stokes Law model this free settling experiment for all concentrations? Explain.
5. Do the setup and procedure accurately imitate free settling of a spherical material? Explain.

References
Yuan, P., & Lin, B. (2008, October 27). Measurement of Viscosity in a Vertical Falling Ball Viscometer.
Retrieved January 31, 2016, from http://www.americanlaboratory.com/913-Technical-Articles/778-
Measurement-of-Viscosity-in-a-Vertical-Falling-Ball-Viscometer/

ChE 135 Laboratory Manual 30


Group Members: _________________________________________ Date &Time
Started:________________
_________________________________________ Date &Time Finished:_______________
_________________________________________ Noted: __________________________
_________________________________________

Viscometry

____________________________________________________________________________________________________

Important Parameters

Wt% (x2) 0% 10% 20% 30% 40% 50% 60%

M2 (g) 100 90 90 70 75 90 100

Density
(g/mL)

Volume of
one glass
bead (mm3) Distance
from A to
Mass of one B (m)
glass bead
(g)

Trial Data

Wt% 0% 10% 20% 30% 40% 50% 60%

Trial 1 (s)

Trial 2 (s)

Trial 3 (s)

Trial 4 (s)

Trial 5 (s)

Trial 6 (s)

ChE 135 Laboratory Manual 31


EXPERIMENT NO. # 8

ANALYSIS OF THE DRYING BEHAVIOR OF DIFFERENT


SOLIDS
Introduction
Drying operations are necessary to achieve the required product specifications in industries such as
pharmaceuticals, food production and paper production. The process of drying primarily involves the
removal of moisture from solids, solutions, slurries and pastes. The rate of drying depends on a number
of factors such as the bulk properties of the material being dried, temperature and humidity. The drying
behaviour of different solids will be observed and analysed in this experiment by establishing their
drying curves.

Objectives, Scope and Limitations


The experiment aims to compare the drying behaviour of three different materials. The materials would
be tested under the same conditions amount of water added, size of container and drying
temperature. The study also aims to identify the different properties that affect the drying behaviour of
a material by observing the drying curves generated for each one. The study will not cover any possible
chemical reactions involved in the process. It will also not tackle separately the contribution to the
drying rate of each type of heat transfer. The study is also limited to the assumption that all the
materials have uniform bulk properties.

Methodology
A. Materials and Apparatus

Distilled water Oven dryer


Grounded charcoal Weighing scale
Sand Aluminum trays
Coffee beans 50 mL graduated cylinder

B. Procedure
1. Turn the dryer on and preheat it to 80C.
2. Weigh and record each empty tray. Measure and record the dimensions of each tray.
3. Place a sample of the material and pour it on a tray. Add 75 mL water.
4. Weigh the tray containing the samples.
5. Put the tray in the dryer after at least 15 minutes of preheating.
6. After every 3 minutes, take out the tray and weigh. Use insulated gloves or mittens when
taking out the sample from the oven. After 10 weights, use intervals of 5 minutes. After
another 10 weights, use intervals of 10 minutes.
7. Monitor and record the weights of the trays with the mixtures for every elapsed time until at
least three consecutive weights are measured or until the initial weight of the dry solid has
been reached.
8. Collect the samples and turn off the dryer. Repeat all steps for each material.

Notes
1. Use oven gloves when removing or putting samples into the oven.
2. The voltage regulator must be turned it before the oven can be used.
3. The temperature control mechanism of the oven is faulty so manual adjustment of the
thermostat must

Guide Questions
1. What properties of the materials affect their drying and how do these properties affect the
drying rate?
2. How do external factors such as drying and humidity inside the oven affect the drying rate?
3. Do the drying curves of the materials exhibit the different drying regimes?

ChE 135 Laboratory Manual 32


References
Foust, A. (1980) Principles of Unit Operations. John Wiley & Sons, Inc., Singapore.
Seader, J.D. (2011) Separation Process Principles. John Wiley & Sons, Inc., USA.

ChE 135 Laboratory Manual 33


Group Members: _________________________________________ Date &Time
Started:________________
_________________________________________ Date &Time Finished:_______________
_________________________________________ Noted: __________________________
_________________________________________

Batch Drying

____________________________________________________________________________________________________

Initial Masses

Material: Material: Material:


Tray Mass (g) Tray Mass (g) Tray Mass (g)
Tray + Dry Tray + Dry Tray + Dry
Material Mass Material Mass Material Mass
(g) (g) (g)
Tray + Tray + Material Tray + Material
Material + + Water Mass + Water Mass
Water Mass (g) (g)
(g)

Drying Data

Material: Material: Material:


Time (s) Mass (g) Time (s) Mass (g) Time (s) Mass (g)

ChE 135 Laboratory Manual 34


EXPERIMENT NO. # 9

DETERMINATION OF THE THERMAL DIFFUSIVITY OF


DIFFERENT SOLIDS
Introduction
Thermal diffusivity is a physical property pertaining to the rate of heat propagation by conduction in a
material during changes of temperature with time. Such property can be used in the analysis and
design of systems subjected to transient temperature changes. In this experiment, the thermal
diffusivity of several solids of cubic geometry would be observed. Several simplifying assumptions
would be implemented to calculate the thermal diffusivity from the temperature profile of the solid.
Newtons law of cooling would be the primary function that would be used to quantitatively analyse the
system.

Objectives, Scope and Limitations


The objective of the experiment is to measure the thermal diffusivity of particular solid samples through
transient temperature measurement. The temperature measurements that would be obtained would
only be limited to the sample core temperature and the water bath temperature. Simplifying
assumptions would also be used to analyse the data that would be obtained.

Methodology
A. Materials and Apparatus

Steel cube with Water bath


thermocouple
Resin cube with Thermometer
thermocouple Stopwatch
Tap water

B. Procedure
1. Measure the sides of the steel cube using a Vernier caliper or a ruler. Do the same for the
resin cube.
2. Fill the constant temperature water bath with tap water up to a level where the steel
cube can be fully immersed. Turn the switch on to start the heating and circulation of
water.
3. Set the water bath temperature to 50oC. Record the initial temperature of both materials.
4. When the water reaches 50oC, submerge the steel cube into the hot water bath. Record
the thermocouple reading every 10 seconds until the temperature reaches that of the
water or until the temperature reading becomes constant. Do the same for the resin
cube.
5. Adjust the temperature to 20oC. Repeat step 4 for the new temperature.
Notes
1. Replace the water in the constant-temperature water bath with tap water to hasten the cooling.
You may also opt to add ice for the water to cool faster.
2. Measurement on the steel and resin cubes can be performed simultaneously provided that there
is enough thermocouples.
3. Make sure that the thermocouple handsets being used are compatible with the rods embedded
in the sample cubes.
4. Empty the water bath after use.

Guide Questions
1. How do the heat penetration curves for the steel and resin samples compare with each other?
2. What are the implications of the assumptions used to treat the data?

ChE 135 Laboratory Manual 35


3. How do the calculated values compare with literature values for the thermal diffusivity of the
two materials?
4. Should there be difference in the heating and cooling curves of the materials?

References
Geankoplis, Christie J. (1993). Transport Processes and Unit Operations 3rd edition. Prentice-Hall
International, Inc: USA.
Wilson, J. (2007). Thermal Diffusivity. Retrieved from http://www.electronics-
cooling.com/2007/08/thermal-diffusivity/.

ChE 135 Laboratory Manual 36


Group Members: _________________________________________ Date &Time
Started:________________
_________________________________________ Date &Time Finished:_______________
_________________________________________ Noted: __________________________
_________________________________________

Thermal Diffusivity

____________________________________________________________________________________________________

Initial Dimensions

Steel Cube Resin Cube


Length of side (cm): Length of side (cm):

Heating Measurements
Initial Steel Cube Temperature (oC): ____________ Initial Resin Cube Temperature (oC): ____________

Steel Cube Resin Cube


Time (s) Temp (oC) Time (s) Temp (oC)

Cooling Measurements

ChE 135 Laboratory Manual 37


Initial Steel Cube Temperature (oC): ____________ Initial Resin Cube Temperature (oC): ____________

Steel Cube Resin Cube


Time (s) Temp (oC) Time (s) Temp (oC)

ChE 135 Laboratory Manual 38


EXPERIMENT NO. # 10

THERMAL RADIATION
Introduction
Thermal radiation is the heat transfer involving electromagnetic waves. It is usually observed with high
temperature systems. Application of thermal radiation concepts can be found in the design of systems
such as fired heaters and heat exchangers. The Stefan-Boltzmann Law is among the fundamental
equations that can be used to describe heat transfer by radiation.

= (r4 4 )

where qb is the rate of radiation emitted by the black body per unit area, is the Stefan-Boltzmann
constant (5.6703 10-8 W/(m2 K4)), and Tr and Ts are the absolute temperatures of the radiator and
the surroundings, respectively. The equation for the Stefan-Boltzmann Law can further be modified by
including a view factor that account for the geometry of the heat transfer.

In this experiment, the heat transfer via radiation from an approximated black body source will be
observed. The effect of other factors such as geometry, temperature, distance and shielding will also be
observed.

Objectives, Scope and Limitations


The objective of the experiment is to observed heat transfer by radiation from a particular source and
how it is affected by factors such as geometry, source temperature, receiver distance and shielding.
The heated plate is assumed to be an object approaching black body behavior. It is also assumed that
the black plate and the heat source are in the state of thermal equilibrium

Methodology
A. Materials and Apparatus

5x 5aluminium foil sheet Thermal radiation setup


5x 5styrofoamsheet
5x 5roof insulation sheet

B. Procedure

Fig 7. Thermal radiation setup

Thermal radiation set-up


1. Make sure that the voltage adjustment knob points at the minimum voltage supply.
2. Insert the plug of the heat source into the electrical socket then turn the power switch on.
3. Loosen the stopper located under the mounted black plate set-up. Horizontally slide the set-
up such that it is 50 mm away from the heat source.
4. Loosen the stopper under the radiometer. Horizontally slide the radiometer so that it is 400
mm away from the black plate.
5. In between the black plate and the radiometer is the aperture holder. Loosen the knobs that
secure the plates and remove the two plates.

ChE 135 Laboratory Manual 39


Effect of temperature
1. Make sure that the radiometer shield is firmly placed on the radiometer.
2. Set the voltage to of the maximum. That is, rotate the voltage adjustment knob 45o
clockwise. Note 1.
3. Record the temperature reading.
4. Record the radiometer reading. This value serves as the ZERO OFFSET.
5. Remove radiometer shield. Note 2.
6. Record radiometer reading
7. Repeat steps 2 - 6 for trials 2 and 3.
8. Set the voltage to of the maximum. That is, rotate the voltage adjustment knob 45o
clockwise. Note 1.
9. Repeat steps 3 - 7 for of the maximum voltage value and to for the maximum value.

Effect of aperture width


1. Make sure that the radiometer shield is not attached to the radiometer. Note 2.
2. Horizontally slide the holder such that it is 250 mm away from the heat source.
3. Make sure that the voltage is in maximum value.
4. Record the temperature and radiometer readings. These are the maximum temperature and
radiometer reading values.
5. Attach the aperture plates on the aperture plate holder and rotate the knobs that secure the
plates to make them upright.
6. Adjust the aperture plates such that there is no space or gap between them. Note 1.
7. Attach the radiometer shield. Note 2.
8. Record radiometer reading. This values serves as the ZERO OFFSET
9. Remove the radiometer shield. Note 2.
10. Record radiometer reading.
11. Repeat steps 7-10 for trial 2 and 3.
12. Adjust the distance between the aperture plates to 10 mm (use a ruler)
13. Repeat steps 7 - 11.
14. Adjust the distance between the aperture plates by an increment of 10 mm until the gap
reaches 30 mm. Per adjustment, repeat steps 7 - 11.

Effect of shielding
1. Make sure that the voltage is in maximum value.
2. Remove the aperture plates. Make sure that the holder is still 250 mm away from the heat
source.
3. Make sure that the radiometer shield is attached to the radiometer. Note 2.
4. Place the styrofoam sheet on the aperture plate holder. Note 2.
5. Record the radiometer reading. This serves as the ZERO OFFSET.
6. Remove radiometer shield. Note 1.
7. Record the radiometer reading.
8. Repeat steps 5 - 8 for trials 2 and 3.
9. Change the styrofoam sheet to the car insulator and aluminum foil. Per change in shielding,
repeat steps 3-8.

Effect of distance between the black plate and the radiometer


1. Make sure that the voltage is in the maximum value
2. Make sure that the radiometer shield is detached from the radiometer
3. Record the radiometer reading
4. Change the distance between the black plate and radiometer by horizontally sliding the latter
by 100 mm away from its original position (also, away from the black plate). Note 1.
5. Record the radiometer reading
6. Repeat steps 4 - 6 for increments of 100 mm until the distance of the radiometer from the
black plate is 600 mm.

After the experiment


1. Slowly turn the voltage adjustment knob clockwise until the minimum voltage is reached.
2. Remove the plug of the heat source from the electrical socket.
3. Put back the aperture plates on the aperture holder.
4. Put all combustible materials away from the heat source.

ChE 135 Laboratory Manual 40


Notes
1. Waiting time for the temperature to stabilize after changing voltage is approximately 10 - 15
minutes.
2. After removal/re-attachment of radiometer shield, wait for approximately 10 - 15 minutes for the
temperature reading to stabilize.
3. When using the aperture plate, make sure that the silver surface faces the heat source.
4. The radiometer sensor surface is 65 mm from the centre line of the radiometer mounting rod.

Guide Questions
1. How does each of the tested parameters affect the rate of heat transfer from the source to the
receiver?
2. How good is the fit of the data with the function of the Stefan-Boltzmann Law?
3. What are the potential causes of deviation from the theoretical values?

References
Foust A, Wenzel L, Clump C, Maus L, Andersen L. (1960) Principles of Unit Operations. 2nd ed.
Singapore: John Wiley & Sons, Inc.
Cengel Y, Ghajar A. (2015) Heat and Mass Transfer: Fundamentals & Applications. 5th ed. New York:
McGraw-Hill Companies, Inc.

ChE 135 Laboratory Manual 41


EXPERIMENT NO. # 11

PRESSURE DROP ACROSS A PACKED COLUMN


Introduction
Gas absorption is an extensively used mass transfer unit operation in the industry. There are
numerous process applications where certain components need to be selectively removed from a gas
stream. McCabe, Smith, and Harriot (1993) refer the commonly used equipment in this process as the
packed tower/column. It consists of a cylindrical column filled with various inert solid objects called
packing material. A liquid inlet and distributor is installed at the top of the column while a gas inlet is
located at the bottom. The tower is run with the liquid flowing down, wetting the packing and the
solute-containing gas flows upward, countercurrent to the flow of liquid. This configuration encourages
intimate contact between the phases, ensuring mass transfer.

According to Green and Perry (2008), one of the earliest materials--first generationused for random or
dumped packing are Raschig rings (Random Packings section, para. 1). These are pieces of tube of
approximately equal length and diameter. Foust, Wenzel, Clump, Maus and Andersen noted in 1980
that Raschig rings are widely used as packing material in the process industries due to its low cost (p.
385). The performance characteristics of packing materials, like those of Raschig rings, according to
Kolev (2006) are as follows:

pressure drop;
loading and flooding point;
liquid holdup;
effective surface area; and
gas- and liquid-side controlled mass transfer coefficient (p. 101).
In this experiment, the performance characteristics of dumped Raschig ring packing are
determined. Pressure drops across the column are measured for both dry packing and irrigated packing.
Measurements for the irrigated packing are carried out at constant liquid flowrate with changing gas
flowrate. From these, data for the loading and flooding points are obtained.

Objectives, Scope and Limitations


Determine the effect of varying fluid flow rates on the pressure drop across a dry column, and a wet
column.

Methodology
A. Materials and Apparatus

Gas-liquid absorption equipment Water

B. Procedure
a. Effect of Air Flow Rate on the Pressure Differential across Dry Column
1. The column must first be completely dried by passing the maximum airflow until all
evidence of moisture in the packing and column has disappeared. This may be performed
a day before the scheduled laboratory class.
2. Connect the column top and bottom to the water manometer with stopcocks labelled S1
and S2.
3. Take manometer readings of pressure differential across the column for a range of airflow
rates (in mm H2O).

b. Effect of Air Flow Rate with Different Water Flow Rates on the Pressure Differential Across the
Column
1. Switch on the water pump and set C1 to give a flow rate,
e.g. 3 L/min.
2. After about 30 seconds close C1, switch off the pump and
allow the column to drain for 3-5 minutes.

ChE 135 Laboratory Manual 42


3. Measure the air pressure differential across the wet column
as a function of the air flowrate.
4. Measure the air pressure differential across the column as
a function of the airflow rate for different water flow rates up to 5 L/min., noting the
appearance of the column at each setting.

Notes
1. Familiarize yourself with the manometers, where they are tapped and what pressure is being
measured.
2. Verify the given pressure scale in the manometers.
3. Do not allow water to reach the tubing for the manometers.
4. The range of possible air flow rates will decrease with increasing water flowrate due to the onset
of flooding on the column, which should be noted. If flooding takes place at a certain liquid flow
rate, stop immediately and do not operate further at higher water flow rates.
5. The minimum air flowrate that should be used in the experiment is 80 L/min.

Guide Questions
1. How does the airflow rate affect the pressure drop across the dry column?
2. Compare the effect of airflow rate for a dry column and for wet column.
3. What is loading point? What is flooding point? And how are these related to the pressure drop in
the column?
4. Is the measured pressure drop consistent with theory?
5. What are the common problems encountered in the operation of the gas absorber column? How
can these problems be remedied?
References
Foust, A. S., Wenzel, L. A., Clump, C. W., Maus, L., & Andersen, L.B. (1980). Principle of unit
operations (2nd Ed.). Singapore: John Wiley & Sons, Inc.
Green, D.W., Perry, R.H. (2008). Perry's chemical engineers' handbook (8th Ed.). NY: McGraw-Hill
Companies, Inc.
Kolev, N. (2006). Packed bed columns for absorption, desorption, rectification and direct heat transfer.
Amsterdam: Elsevier.
McCabe, W. L., Smith, J. C., & Harriot, P. (1993). Unit operations in chemical engineering (5th Ed.).
Singapore: McGraw-Hill Book Co.

ChE 135 Laboratory Manual 43


Group Members: _________________________________________ Date &Time
Started:________________
_________________________________________ Date &Time Finished:_______________
_________________________________________ Noted: __________________________
_________________________________________

Pressure Drop across a Packed Column

____________________________________________________________________________________________________

Water Flowrate 0 L/min 2 L/min 3 L/min 4 L/min


Air Flowrate ___ H1 __ H2 __ H1 __ H2 __ H1 __ H2 __ H1 __ H2 __
80
90
100
110
120
130
140
150
160
170
180

ChE 135 Laboratory Manual 44

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