Chemical Engineering

Unit Operations Experimental Design and Analysis

0906.403

Laboratory Manual

Department of Chemical Engineering

Fall 2016

Table of Contents
General Information.

Point Grading. 2
Laboratory Operation and Safety 3
Signature Sheet.

Permission to Start Laboratory 9

Written Report Guidelines. 10
Grading Sheet 12
Description of Grading .13
Report Checklist 14
Peer Rating Form.. 15
Appendix: Unit Operation Experiments16

Unit Operations Experimental Design and Analysis

0906.403
COURSE AND REPORT PROTOCOL:
The course work will consist of three experiments and in-class workshops. Students will work in groups and
each project will require a group report. Each group will submit a report for each experiment. Plagiarism of
laboratory data or reports will result in academic misconduct charges There will be two exams throughout
the semester. Homework will be assigned during the semester. It is important to be prepared for the
laboratory experiments and to complete any preliminary calculations necessary prior to operating any
equipment. The final grade for the course is composed of laboratory reports, exam and homework grades and
laboratory performance. Peer evaluations will be conducted at midterm and the end of the course, but only the
end-of-course peer evaluation will be included in the final grade. Please note that this evaluation is a significant
contribution to the final numerical score.

VIOLATIONS OF SAFETY AND LABORATORY PROCEDURES

All students must adhere to the laboratory safety rules. Any unsafe practice will result in a deduction of up to 30
points from the final report grade of the laboratory experiment during which the violation took place.
Equipment operating ranges are listed in experimental descriptions. Operation of equipment at
conditions outside the specified ranges will result in a zero (0) grade for the experiment.
Major safety violations or damage resulting in inoperable equipment will result in dismissal from the laboratory
and a zero grade for the experiment.
LABORATORY READINESS ASSESSMENT PRESENTATIONS
Before beginning an experiment, each member of the team must be familiar with the equipment and well versed
in the theory behind the experiment. Laboratory instructors or graduate assistants will check with each group
prior to the start-up of any equipment and assign a laboratory readiness grade.
LABORATORY REPORTS
Each group will write three reports and one standard operating procedure (SOP). Reports should be at most 10
pages in length (excluding appendices, title page, table of contents and letter of transmittal). Microsoft Word
must be used for all reports. Paragraphs must be single spaced and a font size of 12 must be used for the body
of the report. Margins must be at least 0.5 in. and appropriate. A hardcopy and an electronic copy of the report
must be submitted by the report due date. Reports that do not follow the page length, font, spacing and general
format will not be graded.
POINT GRADING
Each assignment will be graded according to the point system below. The final grade will be computed
according to the University grading system as outlined in the Course General Guidelines and Syllabus
distributed in class. There are no make-ups for missed in-class workshops.

POINT GRADING:
Maximum
Number of Points

TASK
Laboratory Readiness+
Presentations

170 (50 experiment 1, 60 each for

experiments 2 and 3)

Laboratory Report 1

200 + 30 for oral

Laboratory Report 2

400 + 60 for oral

Laboratory Report 3

600 + 90 for oral

Professional Conduct
and Peer Evaluation

200

Workshops

300

TOTAL

2050

(+) Theoretical knowledge, command of experimental protocols, laboratory datasheets

Laboratory Safety
Good laboratory technique is not only an essential aspect of professionalism, but also makes it possible to
avoid most accidents. Good techniques include proper handling of chemicals, glassware and apparatus, and the
knowledge of, and habitual use of, safety precautions. Also, good judgment is a key element in laboratory
safety.
GENERAL SAFETY RULES
1. The written approval of the instructor is required for anyone to be in the laboratory after hours (6:30 p.m. to
8 a.m.), on weekends, or on non-scheduled laboratory days.
2. No equipment is to be operated until the approval of the instructor has been obtained at the start of class.
Only the equipment pertaining to the assigned experiment is to be operated. All members of a group are to
be properly informed on the safety aspects of their assigned experiment and to be familiar with the safety
aspects of surrounding experiments
3. Safety glasses with side shields or safety goggles (when handling hazardous chemicals) are required.
Neckties, dangling clothing, jewelry or hair, and other unsafe items are prohibited. Long pants and closed
shoes are required.
4. Sleeping is prohibited in the laboratory. Violation of this rule will result in dismissal from the laboratory for
that day and an unexcused absence.
5. Horseplay of any sort is absolutely prohibited in the laboratory.
6. Smoking and open flames are prohibited in the laboratory.
7. The safety precautions in the experimental plan must be followed.
8. No operating equipment may be left unattended. At least two members of the group must be present while
the equipment is operating.
9. The laboratory floor must be kept dry, clean, and uncluttered at all times. Any spills should be cleaned up
immediately.
10. All chemicals must be transported in a safety carrier. All mercury and alcohol thermometers and more than
one item of glassware must be transported in a bucket or other suitable container.
11. CHEMICALS AND GLASSWARE ARE NOT TO BE TRANSPORTED ON THE SPIRAL STAIRCASE.
12. Students are expected to be familiar with the safety aspects of all the chemicals used in the laboratory and
with the coding system used to label containers and pipelines.
13. Any accident or hazardous situation must be reported to the Laboratory Supervisor immediately.
14. Any serious violation of any of these safety rules may lead to immediate dismissal from the course. Minor
violations of any of these rules will be dealt with in a manner consistent with the Safety Program. A person
3

who repeatedly disregards the safety rules may be dismissed from the course or from specific laboratories
with negative impact on course grade and/or academic standing.

PERSONAL PROTECTIVE EQUIPMENT

Personal protective equipment shall be provided, used, and maintained in a sanitary and reliable condition
whenever it is necessary by reason of process or environmental hazards.
1. DUST MASK
A. A dust mask should be worn when handling powdery solids.
B. Dust masks prevent inhalation of solid particles.
1. EAR PROTECTION
A. Earplugs protect the ears against high-decibel noise (90 dBA or above).
B. If your ears are sensitive to noise, you may want to wear earplugs while working in the laboratory.
3. EYE PROTECTION
A. Safety glasses with side shields or safety goggles are to be worn at all times in the laboratory.
B. Safety goggles must be worn when handling hazardous chemicals.
C. Contact lenses are strongly discouraged in the laboratory. If contact lenses are worn, safety goggles are
strongly recommended in place of safety glasses with side shields.
4. FOOTWEAR
A. The following footwear is not allowed:
1. Ventilated shoes.
2. Sandals.
B. The following shoes are not recommended:
1. Porous leather or cloth shoes.
2. Tennis shoes.
5. GLOVES
A. Insulated gloves are required to avoid burns when operating steam valves and when handling hot objects.
B. Rubber or other protective gloves are required to avoid contact with chemicals that can burn or penetrate
the skin
6. CLOTHING
A. Long pants must be worn in the laboratory (short pants and skirts are not allowed)
B. No neckties, no dangling clothes nor dangling jewelry.
C. Buttoned long sleeve shirts (recommended).
D. Long hair must be held back away from face and laboratory equipment.
E. Long-sleeve laboratory coat must be used when handling chemicals that can burn the skin or be absorbed
through the skin.

7. LOCATION OF PERSONAL PROTECTIVE EQUIPMENT

A. Dust masks, ear plugs, safety glasses and gloves are in the Laboratory.
B. Goggles can be purchased from the B&N Rowan University Bookstore.
4

GENERAL EQUIPMENT SAFETY

1. CHEMICAL SAFETY
A. A safety carrier is available from the Laboratory Coordinator.
B. Transport all chemicals using a safety carrier. The chemical must be in a closed container.
C. NO CHEMICALS are to be carried on the spiral staircase. Use the elevators or alternative stairways.
D. Flammable, volatile chemicals are to be stored in the Flammable Liquids Storage Cabinet.
E. Chemicals are NOT to be stored in the hoods. Chemicals must be removed from the hoods at the end of
the day.
F. Use a Class B Fire Extinguisher for chemical fires.
G. All containers must be labeled as to their contents and must have a Right to Know Law Label attached.
Any unlabelled container must be reported to the Laboratory Supervisor and be treated as a hazardous
substance.
H. Wear protective gloves and apron when handling strong acids and bases.
I. The Laboratory Supervisor must be notified of any new chemical introduced into the laboratory so that
the MSDS can be obtained and all students can be trained on the handling of the chemical.
2. CHEMICAL STORAGE CABINET
A. No flammable, volatile chemicals are to be stored.
B. Store acids and bases on the lowest shelf with acids on one side and bases on the other side.
C. Store oxidizable materials away from acids and bases.
D. ALL chemicals must be labeled.
E. The Laboratory Supervisor must be notified of any new chemical placed in the chemical storage cabinet
so that the MSDS can be obtained and the chemical list updated.
3. ELECTRICAL SAFETY
A. Use the left-hand rule in operating power boxes, i.e. use the left hand to move the handle up or down.
B. Power must be off before making electrical connections.
C. Avoid splashing or spraying water on electrical connections, wall sockets, and junction or power boxes.
D. Keep extension cords away from traffic and water.
E. Use 3-pronged plugs with a ground connection.
F. Use a Class C Fire Extinguisher if energized electrical systems are involved.

4. FLAMMABLE LIQUIDS STORAGE CABINETS

A. Only flammable chemicals may be stored here.
B. Separate incompatible chemicals.
C. ALL chemicals must be labeled.
D. The Laboratory Supervisor must be notified of any new chemical added to the Flammable Liquids
Storage Cabinet so that the MSDS can be obtained and the list updated.

5. FLAMMABLE WASTE CONTAINER

A. A Flammable Waste Container is located in the laboratory for the disposal of solid flammable waste.

6. GAS CYLINDERS
A. Cylinder contents are under pressure; keep cylinders upright and secured to a sturdy base with a chain.
B. The gas or liquid contained in the cylinder should be clearly identified on the container.
C. If a cylinder has been emptied, clearly label this information on the container.
D. Keep the valve cover screwed securely on top of the cylinder while storing.
E. Store cylinders away from high temperatures.
F. Do not store flammable materials near oxygen cylinders.
G. Always move a cylinder tank with a cart; cylinder must be chained to the cart and valve cover screwed
on.
H. Have the Laboratory Supervisor or maintenance personnel change cylinders.
I. Once the cylinder is installed:
1. Make sure connecting pipes and hoses are tight and in good condition to prevent leakage.
2. Check for leaks with soapy water or Snoop.
J. Fully open main cylinder valve.
7. GLASSWARE
A. Glassware is not to be transported up or down the spiral staircase. Use the elevators or stairways.
B. Glassware and mercury or alcohol thermometers must be transported in a bucket or suitable container.
C. Use hand protection when inserting glass tubing into rubber stoppers, corks, or rubber tubing.
D. Glass tubing should be fire polished and lubricated before insertion into rubber stoppers or rubber
tubing.
E. Always wear eye protection when using glassware.
F. Take care in storing and in handling glassware.
G. Discard or replace damaged glassware.
H. Use only vacuum designed glassware for vacuum purposes.
I. Dispose of broken glass in the broken glass container.
8. LADDERS
A. Ladders are always to be chained when not in use.
B. When one or more ladders are in use, the remaining ladders should be chained. A hook on the chain
makes it possible to chain the ladders without locking the chain.
C. Do not use the top two steps and do not lean while using a ladder. Someone should hold the base of the
ladder while it is being used.
D. Avoid lights and electrical wires while moving a ladder.
E. Moving ladders longer than 6 feet requires two people.

9. MANOMETERS
A. By-pass valve must be open before opening valves in lines to manometer legs.
B. Open valve to low pressure source first and then valve to high pressure source.
C. Close by-pass valve slowly and observe manometer reading. If manometer level is going off-scale,
quickly open by-pass valve.
D. Open by-pass valve immediately after taking the reading.
E. Close valve to high pressure source first and then valve to low pressure source.

10. MIXING AND STIRRING DEVICES

A. Keep hands, hair, and loose clothing away from agitator.
B. Lock out the power supply to the agitator before adding material to the tank or before manually stirring
the material in the tank.
C. For hand-held agitators, make sure agitator is off before adding material to the tank.
D. If solids have settled to the bottom of the tank, they should be stirred by hand before starting the
agitator.
E. Make sure the agitator is immersed in the solution to be mixed before starting motor.
F. Turn off motor before removing the agitator from the mixed solution.
11. PERSONAL HYGIENE PRACTICES
A. Wash hands before and after running an experiment.
B. Wear gloves appropriate for the experiment. Clean the gloves after using them.
C. Cover any cuts or open wounds with clean, suitable material.
D. Do not apply cosmetics, skin creams or other body products while in the laboratory.
E. Do not eat in the laboratory area.
F. Keep extra clothing available so that you can change after working in the laboratory or in case your
clothes become contaminated.
G. Do not use your mouth to pipette.
12. PUMPS, FANS, BLOWERS, AND COMPRESSORS
A. Make sure that guards on moving parts and on electrical connections are in place.
B. Keep clothing, hands, and hair away from moving parts.
13. ELECTRONIC DEVICES
A. Operation of electronic devices is only permitted as part of laboratory operation or experiment
execution
14. SAFE LIFTING PRACTICES
A. Clear a pathway before moving things.
B. Check the objects weight to see if help is needed.
C. Keep back straight and vertical to the ground. Keeping your head up and looking straight ahead will
help.
D. Bend knees when lifting; use the legs to lift and not the back.
E. Bring the object as close to the body as possible.
F. Be careful when putting the object down; follow the same guidelines as for lifting.
15. STEAM AND CONDENSATE LINES
A. Use insulated gloves for operating steam valves.
B. Open valves slowly and only to the desired position.
C. Keep hands and clothing away from steam lines.
D. Lines from steam traps should extend into the drain.
E. During initial start up, by-pass steam traps until live steam exits from discharge line.
F. Stay clear of condensate/steam discharge lines, especially during initial start up.

Unit Operation Laboratory

0906.403
I have read the Laboratory Safety section of the U.O. L. Manual and understand the contents. I shall conduct
myself in a safe and professional manner during the time I am in the laboratory and shall notify the Instructor of
any unsafe condition that comes to my attention.
Date: ________________

Signature: _______________________
Printed Name: ____________________

Safety Procedures for Unit Operations Laboratories

PERMISSION TO START EXPERIMENTATION

Experiment Subject/Title:_____________________________________________________
Experiment______________________________________________________
date

time

Operating procedures approved by (initial if OK):

startup
data collection
shutdown
emergency shutdown

Assignments:
data collection plan
safety
operating procedures
data collection/recording
calibration procedures/data
theory

INSTRUCTOR
____________
____________
____________
____________

Student Responsible:
____________________________
____________________________
____________________________
____________________________
____________________________
____________________________

Potential electrical hazards

yes
no
If yes, identify location:
___________________________________________________________________
___________________________________________________________________
Potential mechanical hazards?

yes

no

If yes, identify location:

Required chemicals/physical state/purity/amounts:

___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
MSDA reviewed ______________________________________________________
signature of safety director for group/team

date

Hazardous/toxic chemicals involved?

yes
no
identities:
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________

Written Report Guidelines

Reports should be at most 10 pages long (excluding appendices, letter of transmittal, title page and table of
contents). The object of each report is to present data in a clear manner that can readily be understood by your
peers, instructors and future employers. The reports should be written in the third person, and the tense, at least
in any single paragraph, should be consistent. Grading guidelines are included to help you understand the
grading criteria.
Report Format
a. Letter of Transmittal
b. Title Page
c. Abstract
d. Table of Contents
e. Introduction and Theory
f. Experimental Design and Data Analysis Procedures
g. Apparatus and Operating Procedures
h. Results and Discussion
i. Conclusions and Recommendations
j. References
k. Appendices
a. Sample calculations
b. Raw data and intermediate calculations worksheets
c. Report grading sheet (p. 12 of this document)
The Results and Discussion Section must include an error analysis whenever possible.

Some general report guidelines

Graphs: Graphs should be computer generated. The variables or functions plotted on the axes as well as any
parameter should be shown with the units designated.
Like drawings, graphs should be self contained, i.e., their full meaning should be evident without reference to
the remainder of the report. Thus, all graphs must have a figure number, and an explanatory legend. If more
than one curve is drawn on a single graph, each one must be clearly labeled. When different symbols (circle,
square, etc.) are used to label multiple curves on one graph, symbols must be defined in a key. Colors may be
used to differentiate different curves but must be suitable and clear for black and white copies.
10

Equations: All equations should be generated using Microsoft equation editor, centered, and numbered (with
the equation number flush with right-hand margin).
Note: All equations, tables and figures presented throughout the report are to be numbered. Tables and figures
must have titles.
Key grading points:
Below are some of the elements that will be addressed in grading.

Summary or Abstract: Brief (no more than 2 paragraphs), includes the purpose, experimental technique,
the range of parameters investigated, and main results.
Required items completed: Check protocols for each laboratory for required data and analysis.
Adequate data: Did you gather data in an appropriate range? Was your experimental design appropriate?
Explanation/justification: Are your data reasonable? How do your results compare with the literature?
What do your results mean?
Computer work: Statgraphics, Excel or other software output should be located in appendix.
Sample calculations and error analysis: Should be located in appendix and referred to in text.
Appendix and references: Must be clearly labeled and organized, referenced appropriately in text.
Organization and presentation: Report should be of professional quality and easy to read. Graphs and
charts should be integrated into text whenever possible.

11

Grading Sheet: Group (Full) Report

Unit Operations Laboratory - 0906.403
Experiment Title____________________________________ Due Date____________
Group________________________________

Category and Grade Value

Brief Description
Letter of Transmittal
Formal letter including the name and purpose of report,
3%
contact information, any extraordinary findings,
questions/concerns
Title Page
Report title, date, authors and course information
2%
Abstract
A at most two paragraphs synopsis of experiment, results
3%
and conclusions
Table of Contents
A listing with titles and page numbers of sections, figures
2%
and tables.
Introduction and Theory Theory/basis for experiment, description of literature
15%
available, hypothesis of experiment
Experimental Design and Description of experimental design and rationale for
Data Analysis Procedures selection, correct application of techniques and example
10%
results
Apparatus and Operating Detailed description of experiment including analytical
Procedures
methods should be in technical journal format and not in
15%
the format of the laboratory write-up
Results and Discussion
All results, use of tables and figures, reference to previous
20%
sections to explain results, discussion of data relative to
hypothesis, discuss accuracy and significance of results,
discuss experimental error and conclusions drawn
Conclusions and
Complete, but brief, summary of laboratory and results,
Recommendations
discuss recommendations for improvement based on results
10%
and experimental work, (What should next group do to
improve results?)
References
Appropriate references and format, citations in proper
5%
format throughout text.
Appendices
Proper format, appropriate references throughout text,
5%
sample calculations, error analysis, raw data.
Organization and
Report must be well-researched, presented and discussed.
Presentation
Authors must show comprehensive and in-depth
10%
understanding of subject matter
Total
100%

12

Score

Description of Grading
Percent Description
100% Superior work; no improvements needed
95% Excellent work; one or two corrections recommended
Great work; a little more description needed; maybe a
90% calculation error
Good work; grasps the concept, but nothing elaborate;
85% calculation errors
Average work; a couple of technical errors; lacking full
80% descriptions
OK work; one or two conceptual errors; lacking full
75% descriptions
70% Below average work; several technical errors
65% Poor work; several conceptual errors
60% Poor work; several errors, conceptually and technically
50% Made an attempt, but didn't grasp the overall concept
Wrote something just to fill space; or wrote about wrong
25% subject/material
0%
Nothing submitted; or plagiarized material

13

Check List for Laboratory Reports ChE 0906.403, Unit Operations Laboratory
Yes
General
A Appropriate report length
B 11 or 12 point type, single spaced
C Handed in on time?
D Spelling and grammar checked?
E Design question(s) answered
Group Identified properly, names and number on report
F
Graphs
G Is each graph numbered?
H Graphs fully and clearly labeled
Graph axes labels useful (no furlongs per fortnight)
I
Are the units included for each axis?
J
K Are data points differentiated well?
L Line through the points
M Are calculated or theoretical lines shown without data points?
N Is the line of the proper type? (Straight vs. curve?)
O If the slope is shown, does it make sense and is it necessary?
Even decades for a log-log plot
P
Q Is the graph big enough to see easily?
R Are different data series shown clearly?
Charts
Graphs and charts numbered
S
T Charts titled clearly
U Each column clearly labeled
V Significant Figures
Equations
W Symbols for equations defined
X Equations editor used
Y Equations centered and numbered (with number right-justified)
Summary/Abstract
AA No more than two paragraphs
BB Includes the purpose, the experimental technique, the range of the
parameters investigated and the main results.

14

No

PEER RATING OF

LABORATORY TEAM MEMBERS 0906-403

Fall 2016

Name_______________________________________________________
Please write the names of all of your team members, INCLUDING YOURSELF, and rate the degree to which
each member fulfilled his/her responsibilities in completing their team assignments.
The possible ratings are as follows:
Excellent
(10) Consistently went above and beyondtutored teammates, carried more than his/her fair
Very good
(8.5)
Satisfactory (5)
Ordinary
(4)
Marginal
(2)
Deficient
(1.5)
Unsatisfactory (1)
Superficial (0.5)
No show
(0)

share of the load

Consistently did what he/she was supposed to do, very well prepared and cooperative
Usually did what he/she was supposed to do, acceptably prepared and cooperative
Often did what he/she was supposed to do, minimally prepared and cooperative
Sometimes failed to show up or complete assignments, rarely prepared
Often failed to show up or complete assignments, rarely prepared
Consistently failed to show up or complete assignments, unprepared
Practically no participation
No participation at all

These ratings should reflect each individuals level of participation and effort and sense of responsibility, not
his or her academic ability.
Name of Team Member
YOUR NAME

Rating/Comments

Your signature: ________________________________________

R.M. Felder, 1997. Based on the paper presented by Deborah B. Kaufman, Richard M. Felder, Hugh Fuller,
"Peer Ratings in Cooperative Learning Teams," Session 1430, 1999 ASEE Annual Conference.

15

Appendix:
Unit Operations Experimental Design and Analysis
Laboratory Experiments

16