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CHE 331 Chemical Engineering Laboratory

LAB REPORT GUIDELINE


Each group must submit one report for each experiment within the dateline given. All
students need to prepare materials such as A4 paper, some literatures (online sources or
journals) and textbooks regarding to the topics of experiment given.
General format:
- Font type: Times New Roman
- Size: 12
- Spacing: Double spacing except for abstract (single spacing)
- Margins: 2.5 cm (for top, bottom, right and left)
- Paragraph/Text: Justified and continuous. Please do not leave any empty spaces
between sections.
- Section title: ALL CAPITAL LETTERS and BOLD, align title to the left
- Number each page (type)
The general order of the various sections of a full report is set out below (Please refer
appendices for example):

Front Cover
Include:
- Title of Experiment
- Group #
- Group members name and student ID. Please include assignment of member
starting from planner, experimenter, analyzer and consultant.

Lab report evaluation sheet (A softcopy of the evaluation can be found in ilearn
portal CHE 331 in lab report guideline)

Abstract

Table of Contents:
1.0
Introduction
2.0
Objectives
3.0
Theory
4.0
Diagram and Description of Apparatus
5.0
Experimental Procedures
6.0
Results and Discussions
7.0
Sample calculations
8.0
Conclusions and Recommendations
9.0
References
11.0 Appendices

CHE 331 Chemical Engineering Laboratory

SECTIONS IN REPORT
Abstract

Introduction

Objective

Theory

The abstract should contain a brief overview of your


experimental results.
You should include only a brief paragraph of a few sentences
discussing in general the objective, procedures, results and
conclusion of the experiment.
The abstract should contain less than approximately 300
words for laboratory reports. Although abstract appears in the
beginning of the report, it should be written after the rest of
the report has been completed.
The Introduction should include a review of background
literature obtained from textbooks or other certified
resources about the experiment.
Proper citations should be included in this section. However,
you are encouraged to make an effort to put this section into
your own words.
For full marks, you have to expand the introduction from the
manual (e.g definition, application etc).
State the objective(s) of the experiment concisely, in
paragraph form.
Some key verbs that you will use in the objective might
include to investigate, to plot, to measure, or to
compare.
The section should inform the reader precisely why the
project was undertaken.
The objectives stated in the manual should also be expanded
based on what to be determined in result and discussion
section.

In the Theory section, the theoretical information having


specific bearing on the problem is developed from
fundamental relationships or is presented with proper
references/citations to literature sources.

Equations used in later sections of the report should be


developed and discussed here.

All assumptions made in defining the problem and in


developing the pertinent equations should be clearly stated.

The theory provides the basis for the solution of the project

CHE 331 Chemical Engineering Laboratory


problem.

Diagram and
Description of
Apparatus

Experimental
Procedures

Results and
Discussion

Key pieces of equipment should be identified precisely and


described completely the purpose of each equipment used,
with the aid of schematics diagrams and photographs as
required.

A simple, schematic flow diagram of the apparatus is always


essential in explaining the apparatus.

For full marks, students have to draw (computer drawing) the


diagram of apparatus/process flow diagram themselves.

The general procedure and critical aspects of the


procedure (e.g., how steady state was determined) should
be discussed in this section.

Precautions taken to avoid injury to people and facilities


should be discussed in this section.

Procedures may be modified during experiments. Hence,


when writing the report, procedures should be simplified
based on what have been performed in the experiment.

In order to obtain full marks, all procedures should be written


completely including shutdown procedures and are written in
your own words with correct grammar and verb tenses.

Results

Include all raw data table, calculated data tables and graphs
according to the objective. The results in the tables should be
expanded from raw data tables.

Data should be included with correct units. Label the graphs


(axis) appropriately.

All graphs in the experiments should be plotted using


Microsoft Excel. Hand-plotting using graph paper is NOT
allowed.

CHE 331 Chemical Engineering Laboratory

Discussion

Sample
calculation

Conclusion and
Recommendatio
n

References

This section is devoted to your interpretation of the outcome


of the experiment.
The information from the data analysis is examined and
explained. You should describe, analyze and explain (not
just restate) all your results.
This section should answer the question what do the data
tell me? Describe any logical projections from the outcome,
for instance, the need to repeat the experiments or to measure
certain variables differently.
Assess the quality and accuracy of your procedure. Compare
your results with expected behavior/hypothesis, if such a
comparison is useful or necessary, and explains any
unexpected behavior. Discussion should relate back to the
theory and results especially the graphs (if applicable).
Do not forget to report values of results with units (except
constant numbers). Numbers without units are
meaningless!
Provide only one sample calculation for each
equation/formula. All calculations should be typed.
Use equation tools embedded in Microsoft Words when
typing all equations/numbers.

The solution to the objective of experiment, as based on both


theory and on the experimental results, is presented and
evaluated.

Recommendations consistent with the problem solution are


then given.

Students/engineers often have a tendency to give cursory


treatment to this vital report section.

Recommendation should not include any safety precaution or


changes of any equipment. Significance of recommendations
should be elaborated.

Instead, improvement of experimental technique or expand


of knowledge may be provided.

Using standard bibliographic format, cite all the published

CHE 331 Chemical Engineering Laboratory


sources you consulted during the conduct of the experiment
and the preparation of your laboratory report.

Appendices

List the author(s), title of paper or book, name of journal, or


publisher as appropriate, page number(s) if appropriate and
the date.

If a source is included in the list of references, it must also


be referred to the appropriate section(s) in the report.
(Refer format of citations)

All raw data for each experiments as well as the design of


experiment data should be attached here.

Detailed specifications for key pieces of equipment and


information about auxiliary apparatus (specifications,
instrument calibrations, and similar information) should be
placed in the Appendices.

FORMAT IN LAB REPORT


Verb tenses for Formal Technical Reports
The abstract, experimental procedures and results sections should be written in the
past tense as you have already carried out the work. An introduction is usually
written in present tense, because you are writing about facts which are true at the
present time. Most scientific literature is written in the passive voice, not the
active voice (i.e not using the words you, we, I or us):
Passive: Solutions were prepared using 0.1 M HCL
Active: We prepared our solutions using 0.1 M HCL X
Remember to proofread and spell-check your reports!

Format for diagrams, figures, tables or charts:


Introduction (or other section in report)
E.g Citation in report:
In fluid dynamics fluids are in motion. Generally they are moved from place to place by
means of mechanical devices such as pumps or blowers, by gravity head, or by pressure,
and flow through systems of piping and process equipments [1].

CHE 331 Chemical Engineering Laboratory

In reference sections:
[1]. Author last name, Authors initial. (year). Title of books, Place of publication:
Publisher. Page
Theory
Naming equation:
For example:
The amount of carbon dioxide in water can be calculated based on the following
equation:
Total digit x digit multiplier = mg/L as CO2 .. (1)
This is so that in discussion the equation can be referred as:
By using equation 1, the concentration of Carbon dioxide is 20mg/L.
Avoid writing any equation/formulas in any paragraph as follows:
The concentration of carbon dioxide can be calculated by using Total digit x digit
multiplier = mg/L as CO2
Apparatus
Labeling diagram/figures/charts: Title should be placed at the bottom of diagram

Figure 1: The diagram for the oil platform


Results
Labeling tables: Title should be placed on top of the table.
Do not forget to include units inside tables.

CHE 331 Chemical Engineering Laboratory

Table 1: Range of Carbon dioxide


Range as CO2 (mg/L)
Total digit
10-50
0.2
10-200
0.1

Volume (mL)
10
30

References
All references should be in alphabetical order and follow the appropriate format.
For books:
Blaxter, M. (1976). Social class and health inequalities. In C. Carter & J. Peel (Eds),
Equalities and inequalities in health. London: Academic Press. Page 7-9
Online sources: Please provide a complete web address
Leafy seadragons and weedy seadragons. (2001). Retrieved November 13, 2002, from
http://www.windspread.net.au/~jenny/seadragons/
Journals:
Aksu, Z, and Akpinar, D. (2001). Competetive biosoprion of phenol and chromium (VI)
from binary mixtures onto dries anaerobic activated sludge. Biochemical
Engineering Journal, 7, 183-193
LAB REPORT SUBMISSION:

Submit a complete lab report ONE WEEK after the experimental lab has been
done. Please submit to the instructor in the lab. Report that is not compiled
together will not be accepted.
Report which does not follow the required format will be returned back for
correction, and marks will be deducted.
Planner: To compile all sections, arrange and staple all pages accordingly, and
cover the left side of report with a single sided tape (black color)

CHE 331 Chemical Engineering Laboratory

PLAGIARISM IS A SERIOUS ACADEMIC OFFENCE!


Please be aware that UiTM and Faculty of Chemical Engineering take serious view of
any form of plagiarism in lab report.
If found guilty:
1. Throughout the report section will be given zero (0) marks as penalty/punishment
of plagiarism, REGARDLESS only part of the content were plagiarized.
2. Without proper citations and references also may be penalized as plagiarism.
3. You may be resulted to fail grade of the course.

Revised and updated: 14 March, 2013

CHE 331 Chemical Engineering Laboratory

Appendices

CHE 331 Chemical Engineering Laboratory

LIQUID-LIQUID EXTRACTION

CHE 331 CHEMICAL ENGINEERING LABORATORY

Instructor:
Group:
Planner:
Experimenter:
Analyzer:
Consultant:

Student Name
Student Name
Student Name
Student Name

Student ID
Student ID
Student ID
Student ID

Date of experiment performed: September 21, 2005

CHE 331 Chemical Engineering Laboratory

CHEMICAL ENGINEERING LABORATORY REPORT EVALUATION SHEET


TEAM:
EXPERIMENT:
PLANNER NAME:
SCOPE

CRITERIA

FULL
MARKS

Introduction

General overview about the experiment

Aims/Objectives

Based on experiment in paragraph form

brief summary from the theory given; add additional data from resources

10

Theory

MARK
S

Total:
Checked by:
EXPERIMENTER NAME:
SCOPE

CRITERIA

FULL
MARKS

Diagram and Description


of Appratus

include the description of main apparatus, as well as sketched diagram

Methodology/Procedure

simplified procedures based on what have been done in the lab

10

Reference/Appendix

extra information extracted/gathered from books/journal


complete raw data and appendices

5
Total:

Checked by:
ANALYZER NAME:

MARK
S

CHE 331 Chemical Engineering Laboratory

SCOPE

FULL
MARKS

CRITERIA
- data must be similar with what that was obtained during experiment (cross check
with raw data given by students)
- produce graph/figures based on the data obtained
discuss what the result & data mean; discuss & relate the results obtained with the
theory

Results
Discussion

MARK
S

20
20
Total:

Checked by:
CONSULTANT NAME:
FULL
MARKS

SCOPE

CRITERIA

Abstract

Must provide the objective of the experiment, procedures, results & conclusion
-

Sample Calculation
Conclusion

Sample of calculation for each variable


Present data accordingly

relate the results obtained with the objective of the experiment


-any improvement to be suggested by observing the inconsistencies observed
in results/conclusion

Recommendation

MARKS

5
5

Total:
Checked by:

Laboratory Session
Rubrics
Mark
distributi
on
Criteria

Set up and
Equipment
Care

Following
Procedure

<50

50-59

60-69

70-79

80-100

Set-up of
equipment is
not accurate,
help is required
with several
major details
Many
necessary
supplies must
found in midlab

Set-up of
equipment is
generally
workable with
several details
that need
refinement.
Some
necessary
supplies must
be searched
out.
Demonstrates
general
knowledge of
lab procedures.
Requires help
from lecturer
with some
steps in
procedures.

Set-up of
equipment is
generally
accurate with 1
or 2 small
details that
need
refinement
All necessary
supplies on
hand

All equipment
accurately
placed
All necessary
supplies on
hand

All equipments
accurately
placed
All necessary
supplies on
hand
Very neat and
organized

10

Demonstrates
good knowledge
of the lab
procedures.
Will ask peers
for help with
problems in
procedures
Works to
follow each step
before moving
on to the next
step.

Demonstrates
sound
knowledge of
lab procedures.
Will discuss
with peer to
solve problems
in procedures.
Carefully
follows each
step.

Demonstrates
very good
knowledge of
the lab
procedures.
Gladly helps
other students
to follow
procedures.
Thoroughly
and carefully
follow each step
before moving
on next step.

15

Lacks the
appropriate
knowledge of
the lab
procedures
Often requires
help from the
lecturer to even
complete basic
procedures.

Full marks

CHE 331 Chemical Engineering Laboratory

Data
Collection

Safety

Clean - up

Measurements
are incomplete,
inaccurate and
imprecise
Observations
are incomplete
or not included.
Symbols,
units and
significant
figures are not
included.

Measurements
are somewhat
inaccurate and
very imprecise
Observations
are incomplete
or recorded in a
confusing way.
There are 3 or
more minor
errors using
symbols, units
and significant
digits or 2
major errors

Measurements
are mostly
accurate
Observations
are generally
complete.
Work is
organized, only
2 or 3 minor
errors using
symbols, units
and significant
digits.

Measurements
are accurate
with
reasonable
precision.
Observations
are thorough.
Work is
generally neat
and organized.
Include
symbols, units
and significant
digits

Measurements
are both
accurate and
precise.
Observations
are very
thorough and
may recognize
possible errors
in data.
Work is neat
and organized.
Includes
appropriate
symbols, units
and significant
digits.

10

Proper safety
precautions are
consistently
missed.
Needs to be
reminded often
during lab

Proper safety
precautions are
often missed.
Needs to be
reminded more
than once
during lab

Proper safety
precautions are
generally used.
May need to
be reminded
once during lab

Proper safety
precautions are
consistently
used.
Uses general
reminders of
safe practices
independently

Proper safety
precautions are
consistently
Consistently
thinks ahead to
ensure safety
Will often help
other students
to conduct labs
safely

10

Proper cleanup procedures


are seldom
used
Often requires
help to
complete cleanup
3 or more
items left at
station or
station not
cleaned

Needs to be
reminded more
than once
during the lab
to use proper
clean-up
procedures
1 or 2 items
left at stations
or not cleaned

Proper cleanup procedures


generally used
May need
some help on
occasion to
complete some
tasks
Stations
generally left
cleaned

Consistently
uses proper
clean-up
procedures
Station
generally neat
and clean

Consistently
uses proper
clean-up
procedures
Often will help
other students
to complete
tasks properly
Station always
left neat and
clean

CHE 331 Chemical Engineering Laboratory


EXAMPLE OF ABSTRACT
The Uni-Minn Development Corporation was asked by Phillips
Pharmaceuticals to evaluate a bench-scale pulsed column to determine how the
amplitude frequency product (af) and relative flow rates affect the extraction
performance of 5 wt% acetic acid from a continuous aqueous phase to a dispersed
toluene phase. Amplitude was held at a constant 2.25 cm, frequencies were varied
from 17.91 to 41.36 0.5 cycles/min, toluene flow rates were varied from 2.79 to
4.25 0.1 gal/hr and aqueous flow rates were varied from 2.27 to 3.02 0.1 gal/hr.
Amplitude was increased to 2.35 cm for one run at a frequency of 33.17 0.1
cycles/min to compare against a run with equivalent amplitude frequency product.
Titrations were performed to obtain equilibrium data and to determine the
concentrations of the inlet and outlet streams. The equilibrium coefficient was
found to be 0.026 0.018 weight fraction toluene per weight fraction water compared
to a literature value of 0.0364. The number of transfer units (NTU) ranged from 0.17
to 1.72 and the height of transfer units (HTU) ranged from 1.74 to 17.68 0.2 ft.
HTU decreased and NTU increased with increasing amplitude frequency product.
A process to extract 0.5 wt% antibiotic from fermentation broth was designed
utilizing a pulsed column extractor with an amplitude frequency product of 3.05
ft/min. The column is 16.8 ft tall, with an inside diameter of 1.48 feet and flows 200
gal/min in the continuous aqueous phase and 450 gal/min in the dispersed toluene
phase to produce 28,600 4000 kg of antibiotic annually.

Objective

Procedure

Result and
conclusion

CHE 331 Chemical Engineering Laboratory

Table of Contents
Abstract.......................................................................................................................1
Table of Contents........................................................................................................2
1.1

Introduction.................................................................................................................3

2.1

Description of Apparatus............................................................................................9

3.1

Experimental Procedures..........................................................................................10

4.1

Results.......................................................................................................................13

4.2

Calculated Data Tables........................................................................................13

4.3

Final Data and Results........................................................................................17

5.1

Discussion of Results................................................................................................24

6.1

Design Problem.........................................................................................................27

7.1

Conclusion and Recommendations...........................................................................29

8.1

Nomenclature............................................................................................................31

9.1

References.................................................................................................................32

APPENDICES...................................................................................................................33
A.1 Original Data Sheets.................................................................................................34
A.2 Sample Calculations..................................................................................................38
A.3 Design Problem Calculations....................................................................................40
A.4 Error Analysis...........................................................................................................42
A.5 Special Topics Report...............................................................................................44

CHE 331 Chemical Engineering Laboratory


1.1 INTRODUCTION
Liquid-liquid extraction is the process of separating two or more components due to
solubility differences in immiscible liquid phases. A feed solution containing the solute is mixed
countercurrently with a solvent through a series of perforated plates.

Density differences

between the two immiscible liquids results in a liquid-liquid interface. The less dense (light)
phase and the denser (heavy) phase are then separated from each other from the top and bottom
of the column, respectively. This is shown graphically in figure 1.

Light Extract
V2, y2
act

Heavy Feed

L2, x2

Interface

Light
Solvent

V1, y1

Heavy
Raffinate L1, x1

Figure 1.1 Liquid-Liquid Extraction

1.2 OBJECTIVE
The objective of this experiment was to attain the performance characteristics of a pulsed column
extractor in the extraction of acetic acid from the continuous aqueous phase to the dispersed
toluene phase. This was accomplished through the control of two key independent variables: the
volumetric flow rates of the aqueous and toluene phases and the pulse frequency. Evaluating the

CHE 331 Chemical Engineering Laboratory


column at various frequencies and flow rates allowed allows the experimenters to draw
conclusions as to how the two variables affect column performance and thus affect the
subsequent design of an effective pulsed column extractor. It is important to note that pulsed
columns typically outperform conventional packed columns.
1.3 THEORY
The efficiency of an extraction is defined by the ability of a column to effectively transfer solute
from the feed to the solvent. The two values commonly used to quantify column efficiency are
the number of transfer units (NTU) and the height of transfer units (HTU). The number of
transfer units based on the solvent phase can be calculated from the concentrations of solute in
the solvent inlet and outlet, y1 and y2 respectively [1].
NTU

y1 y2
y1 y y2 y2*
*
1

y y
ln
y y

*
1

*
2

101\* MERGEFORMAT (.)

1.4 DESCRIPTION OF APPARATUS


The Pulse Liquid-Liquid Extraction is carried out using a bench-scaled pulse column, shown in
Figure 2.1. The system has six perforated plates made of stainless steel, each drilled with 18 holes
with the size of 1/8 inches diameter. The pulse generator, located at the back of the column has
adjustable amplitude that varies up to 2 inches and operates with frequency ranging from 0 to 42
cycles per minute. The feed rate of toluene can be changed by adjusting V19 and this flow rate
can be measured in R1. The same goes for acid feed which can be set in V12 by adjusting R2. For
the purpose of this experiment, the flow rate should not exceed 4.5gal/hr to prevent flooding.

CHE 331 Chemical Engineering Laboratory

2
3

V13

Acid
Feed
A-1

Legend
1 = 1.5 inch x 3 ft. pyrex pipe
contains 6 plates
2 = 1 inch x 3 inch x 10 inches
pyrex tee
3 = 3 inches x 1ft. Pyrex pipe

V17

Spent
Toluene
T-3

R2
V6

Toluene
Outlet
sample

V12
V11

4 = 1.5 inch to
3 inches x 5 inches
pyrex reducer

Acid inlet
Sample

Toluene
Feed
T-1

Open
Valves

Spent
Acid
A-2

V22

Closed

A Acid Tanks
T
R1

V20

V14

V16
V19

Toluene inlet
Sample

V18

Toluene Tanks

R Rotameters

Acid outlet
Sample

Figure 2.1 Process Flow Diagram


Pulse Extraction Column

1.5 RESULTS AND DISCUSSION


Table 4.2.1: Operating Condition for the Runs
Trial

Run 1
Run 2
Run 3
Run 4
Run 5

Acid
Feed
Reading
(R1)
0.1
2.0
2.0
2.2
3.75
2.7

Toluene
Feed
Reading
(R2)
0.1
2.0
2.0
3.8
2.0
3.4

Pulse
Frequency
Reading
0.
05
0.57
1.25
1.20
1.80
2.40

Calibrated
Calibrated
Acid Feed Toluene
Flow Rate
Feed Flow
Rate
0.1 (gal/h) 0.1 (gal/hr)
2.27
2.79
2.27
2.79
2.46
4.67
3.92
2.79
2.93
4.25

Calibrated
Pulse
Frequency
0.1
(cycles/min)
17.91
23.58
23.14
28.67
34.74

CHE 331 Chemical Engineering Laboratory

Figure 4.3.1: The operating line has a positive slope greater than the slope of the
equilibrium line.

Figure 4.3.8: The points on the graph indicate a concave up trend line with
negative slope.

CHE 331 Chemical Engineering Laboratory


1.6 SAMPLE CALCULATION
Complete Changes of Contents of the Tower

1 ft
1.5in

12in

Volume of Column

3 ft

28.3L
4L
1 ft 3

4L
11 min
gal
1hr
4.56 L
(2.79 2.27)

hr
60
min
1gal
Complete Change of Contents =

DISCUSSION
Plot of Overall Height of Transfer Unit
The plot of the overall height of transfer unit decreases as af (the product of pulse
amplitude and pulse frequency) increases. The slope of a possible trend line also increases with
af causing the trend to be concave up.
These trends were the expected results because the figures in Reference (3) also displayed
similar trends. The calculated height of a transfer unit was higher than expected because the
largest HTU in Reference (3) was 3.3 0.1 ft. and the largest HTU calculated was from run 1, at
17.6 0.2 ft. This discrepancy in numbers is likely due to difference in the equipment used in the
reference and the equipment used to measure the data, however, the graphs still share the same
shape.
The error in the calculated equilibrium value could have been a result of the assumption
that the equilibrium line was linear in the dilute region, the toluene-water mixture not having
been mixed well enough or not been given enough time to reach equilibrium, or an error in
measurement.

CHE 331 Chemical Engineering Laboratory


1.7 CONCLUSIONS AND RECOMMENDATIONS
Conclusions

The height of a transfer unit decreases as af (the product of the pulse amplitude and pulse
frequency) increases and is concave up, decreasing less as af increases.

The error in calculating the HTU is 0.2 ft, with the error in the equilibrium making the
largest contribution to that error.

Recommendations

Cover as broad a range as possible with the pulse frequency and with the ratio of the
aqueous and toluene flow rates.

Measure more samples for the calculation of the equilibrium line.

Measure the toluene phase holdup after each run.

9.1 REFERENCES
(1) Geankoplis, C.J., Transport Processes and Separation Process Principles, 4th ed.,
Upper Saddle River, NJ: Prentice Hall, pp. 795-802, (2003).
(2) Perry, R.H., Green D., Perrys Chemical Engineering Handbook, 7th ed., New York,
NY: McGraw-Hill, pp. 15-4 to 15-20, (1973).
(3) Sege, G., Woodfield, F., Pulse Column Variables, Chemical Engineering
Progress, 50:No. 8, 396-402, (1954).
(4) Treybal, R.E., Mass Transfer Operations, 3rd ed., New York, NY: McGraw-Hill, pp.
502-507, 530-555, (1980).
(5) Woodman, R., The System Water-Acetic Acid-Toluene Triangular Coordinates at
25 C, J. Physical Chemistry, 30, pp. 1283-1286 (1926).

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