LAB MODULE

SMJC 3731
CHEMICAL PROCESS ENGINEERING
LABORATORY 3
(Separation)

Name :
Course :
Semester :
Section :
Group :
Lab :
Coordinator

Department of Chemical Process Engineering

Malaysia – Japan International Institute of Technology (MJIIT)
UNIVERSITI TEKNOLOGI MALAYSIA
KUALA LUMPUR
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Contents
LABORATORY SAFETY, RULES AND REGULATIONS .......................................................................... 3
GENERAL RULES ........................................................................................................................... 3
SAFETY RULES .............................................................................................................................. 3
RESPONSIBILITY OF STUDENTS .................................................................................................... 4
CHEMICAL STORAGE AND HANDLING ............................................................................................. 5
GUIDELINE FOR LAB PROPOSAL ...................................................................................................... 6
GUIDELINE FOR LAB REPORT ........................................................................................................... 7
EXPERIMENT 1: LIQUID-LIQUID EXTRACTION ............................................................................... 10
EXPERIMENT 2: DISTILLATION ....................................................................................................... 15
EXPERIMENT 3: EVAPORATION ..................................................................................................... 20
EXPERIMENT 4: GAS LIQUID ABSORPTION .................................................................................... 25
EXPERIMENT 5: OPEN ENDED – SHORT PATH DISTILLATION ........................................................ 30
APPENDICES................................................................................................................................... 32

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LABORATORY SAFETY, RULES AND REGULATIONS

BASIC PRECAUTIONS

Awareness is the most fundamental rule of chemical safety. Take time to understand the safety and
health hazards of the chemicals in the workplace. Every laboratory worker should take the following
precautions:

GENERAL RULES

 Students must abide the dress code while working in the laboratory.
 Every student must wear lab coats and close toe shoes. Slippers, sandals, high-heel shoes are
prohibited during working in the laboratory.
 Students with long hair must get their hair tied up tidily before and during the experiments.
 Bags and other belongings must be kept at the designated places.
 Eating, drinking and smoking are prohibited inside the laboratory.
 Noise must be kept to the minimum as a courtesy to respect others.
 Students are not allowed to working alone without the supervision of laboratory instructor/officer.
There must be at least 2 person present in the laboratory at the same time.
 All specific safety precautions in the laboratory must be obeyed.
 Any unauthorized experiment without the knowledge of laboratory instructor is prohibited.
 All instrument and equipment must be handle with care.
 Workplace has to be cleaned and tidied up after the experiment completed. All instrument and
equipment must be returned orderly after use.
 Students are prohibited to take any equipment or any technical manuals out from the laboratory
without the permission from laboratory instructor/officer.
 Students need to instil an instinctive awareness towards property value of laboratory equipment
and be responsible when using it. Any damages can cause the failure of individual work but also
jeopardize the university name.
 Students shall be liable for damages of equipment caused by individual negligence. If damages
occurred, an investigation will take place to identify the causes and the names of the involved
students will be recorded for faculty attention.
 Students should report immediately to the laboratory instructor/officer if any injury occurred.
 Reports to laboratory instructor/officer immediately if discovered any damages of equipment or
being in the hazardous situation.
 Please check the notice board regularly and pay attention to laboratory announcements.
 Please check with the laboratory instructor regarding the deadline of laboratory report
submission.
 Disciplinary action shall be taken against those students who are failed to abide the rules and
regulations.

SAFETY RULES
The following housekeeping and hygiene practices should be implemented at all times to reduce
the likelihood of accident or chemical exposure:

General Safety Rules

 It is important for each student to follow the procedures given by the laboratory instructor when
conducting laboratory experiments.

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 It is always a good practice and the responsibility of an individual to keep a tidy working condition
in laboratory.
 Before any experiment starts, students must study the information / precaution steps and
understand the procedures mentioned in the given laboratory sheets.

Safety attire
 Hands should be washed after every experiment, before touching any non-contaminated area
or object, and before leaving the laboratory area.
 Every student must wear proper safety equipment at all the times when running the experiment.
 Students are required to wear googles, gloves, apron and mask when handling corrosive or
active chemical agents.
 Safety helmet must be used if students need to climb; e. g. distillation column to collect data
and record the observation.

Laboratory equipment
 Students are prohibited from using the experimental equipment before receiving the explanation
from laboratory instructor/officer.
 Before using the equipment, make sure appropriate and correct power source for the
equipment.
 Sensitive equipment cannot be removed from the designated area.
 Please report immediately any damages of equipment to the laboratory instructor/officer.

Disposal of Laboratory Waste

 Students are held responsible to cleaning the table area and all equipment that used during the
experiment.
 Wastes must be properly labelled and disposed in a designated area.
 Work areas should be kept clean and free from obstruction.

Electricity, Gas and Others

 All sources of gas, fuel and gas flow valve must be turned off tightly before leaving the laboratory
and whenever not in use. The cover of a fume chamber must be lowered at the lowest level.
 Make sure the right power source is used for the equipment to be engaged. Equipment which
are not in use must be switched off.
 If there is a tingling feel when working with electrical devices, stop and switch off the devices
immediately. Place a warning note before reporting to the laboratory instructor/officer and wait
for further instruction.
 Do not work with electricity under wet condition in laboratory. Electric shock is a serious fatal
error due to human negligence and may cause death.
 Access to exits, emergency exits, aisles, and controls should never be blocked.
 Emergency exits should be kept unlocked from the inside.
 Stairways and hallways should not be used as storage areas.

RESPONSIBILITY OF STUDENTS
 Attendance is compulsory and the attendance shall be taken and please sign it during the
laboratory session.
 Laboratory report only be accepted for submission if the student has attended the laboratory
session.

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 Students must come to the laboratory at least 10 minutes earlier to the laboratory before the
experiments start.
 Student need to be punctual to attend the laboratory session.
 Students who are late more than 15 minutes will be barred from attending the laboratory
session. Only the students with valid reason of medical basis (with MC) or unforeseen
circumstances can be considered to apply for laboratory replacement.
 Students are mandatory to participate in all the outlined experiments. Students are considered
FAIL if the students do not attend even one experiment.
 Students are expected to study the lab manual before the laboratory session start.
 Students are required to read and understand the work procedures and experimental theory
beforehand to ensure the experiment goes smoothly.
 Students must complete the experiment within the allocated duration of laboratory session.
 All students are responsible for the condition of their working area at the end of each laboratory
session. All power of the equipment and instruments should be turned off, and cooling water
flows should be shut off. Glassware used should be cleaned and dried.
 Students have to pass up their experiment results to the laboratory instructor on the same day
after each experiment. A copy of the experimental result with stamp must be attached together
with the laboratory report.
 Students are prohibited to use any communication devices (cell phone, smartphones, personal
computer) during the lab session.
 FABRICATING and PLAGIARISM are strictly prohibited. Strict action will be taken if the
students is found fabricating results or copy from others.
 Students have to pass up their laboratory report 1 weeks after the date of experiment to
laboratory coordinator. The report will be not received by failing doing so.

CHEMICAL STORAGE AND HANDLING

Many potential hazards are associated with the storage and handling of laboratory chemicals.
These hazards may be minimized by understanding the properties of the chemicals and by
developing procedures by which they may be handled safely. Simply storing chemicals
alphabetically is not prudent. Flammable, corrosive, explosive, and peroxide forming agents require
special precautions. Storing incompatible chemicals together may have disastrous results.

The following guidelines are prudent for all chemical storage and handling:

 Chemical handling: Use bottle carriers to transport chemicals. Close caps securely. Pour all
chemicals carefully. Add acid to water, not water to acid.
 Labels: Be sure all labels are securely attached and legible. Keep chemicals in their original
containers if possible. Label all secondary containers to avoid unknown chemicals and/or
inadvertent reaction. Date all chemicals, which may become unstable over time or are
peroxidizable.
 Shelves: Do not store chemicals on hard-to-reach shelves. Labels on stored chemicals should
be able to be read easily. Shelves should be made of a chemically resistant material and should
have a 2-inch lip or side rails.
 Incompatible chemicals: Incompatible chemicals should not be stored together. For each
chemical, the hazardous nature must be considered individually and in relation to other
chemicals in the area.
 Excessive storage: Avoid stockpiling chemicals. Purchase only what is needed. Use older stock
first. Discard chemicals that are no longer needed or that have expired.
 Fume hoods: In general, fume hoods should not be used for storage of chemicals, unless the
chemicals are part of the experiment being conducted in the fume hood at that time. The
exception is storage in a fume hood, which is specifically designed for that storage, and where
experimental procedures are not carried out.

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EMERGENCIES

Be sure you know the location and method of operation of the nearest eye wash, safety shower,
fire extinguisher, spill kit and fire alarm pull station. Be sure that emergency telephone numbers
are posted or otherwise accessible.

 Spill
If flammables are involved, extinguish ignition sources. Clean the spill, only if the spill is
manageable, you have been trained and you have appropriate clean-up materials. If you are unable
or do not attempt to clean the spill, prevent the spread if possible, evacuate the area, close the lab
door, and alert others or sound alarm. Communicate with your supervisor and technicians
immediately.

 Fire
Extinguish the fire if it is small, contained, you have been trained and you have an appropriate fire
extinguisher available. If you are unable or do not attempt to extinguish the fire, pull the nearest fire
alarm and evacuate the building via the nearest exit. Communicate with your supervisor and
technicians immediately.

 Chemical Exposure
o Splash to skin or eyes: flush with water at least 15 minutes using a safety shower or eye
wash and seek immediate medical attention.
o Injection: control bleeding, wash with soap and water and seek immediate medical attention.
o Ingestion: seek immediate medical attention.
o Inhalation: stop emission if possible, alert others or sound alarm, get fresh air and seek
immediate medical attention.

Communicate with your supervisor and technicians immediately for the occurrence of any
emergency cases.

GUIDELINE FOR LAB PROPOSAL

Lab Proposal or lab preparation report is a formal draft of portions of the Final Report. It must be
handwritten and submitted at the end of the lab hours during the lab preparation week for the
corresponding experiments. It should include roughly the introduction, overall methodology,
analysis, experimental plan and anticipated results. Planning for delegation of task (role playing)
when the experiment is in progress must also be included.

The content of lab proposal attests to your understanding of the experiment, its context in theory,
and a suitable approach to performing the experimental work as well analysing the results. A
properly prepared lab proposal will save much time in the later phases of the experiment and will
reduce the chances of errors in data collection and analysis. The lab proposal must be handwritten
and prepared on the experimental sheet. It must be clear, concise and specific, but its specific
contents will depend largely on the actual experimental work that you will be doing. Descriptions
with the assistance of charts and/or diagrams, instead of 100% wordy sentences, are very much
encouraged.

The lab proposal should consist of the following sections:

1. Cover Page
The cover page should be prepared on the given standard template.

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2. Introduction
This section should cover the background of the experiment under investigation. There is a brief
explanation on the problem statement, objective of experiment, scope of experiment and the
significance of experiment in the context of knowledge and its application.

3. Methodology
Overall methodology should outline the planning of the whole learning process in order to
accomplish the experiment. Flow chart of overall methodology can be presented in this section.
You should also include roughly the experimental procedures and associate the description with
suitable illustration.

4. Experimental Plan
Basically, experimental plan identifies the list of data/information needed and variables to be
investigated along with their methods of measurement. In addition, any essential data that can be
obtained before doing the experiment must be identified and put in this section.

You should also include the outline of team plan in order to accomplish the experiment, and the
statement of task delegation among the team members before, during and after the experiment.

5. Anticipated Results
Briefly discuss the relevant anticipated results and the manner in which you intend to present them.
Prepare sketches of tables or figures with the expected trends and justify them. Discuss why you
anticipate these results.

GUIDELINE FOR LAB REPORT

Basically, your Final Lab Report should tell what you did, why you did it, what you learned and the
significance of your results. The report does not have to be extremely long. In fact, the key to
writing an excellent report lies in presenting concisely your response to the objectives of the project
and justifying that response with appropriate documentation. The final lab report should consist of
the following sections:

1. Cover Page
The cover page should be prepared on the given standard template.

2. Introduction
Pertinent background and explanatory information about your experiment must be presented if your
audience is to ‘connect the dots’ of later sections of your report. Introduce the objective of
experiment, scope of experiment and the significance of experiment as what you have done in your
Lab Proposal with the necessary improvement.

3. Literature Review/Theory
The literature review and/or theory section is a brief review of relevant ideas from the major field
and a more intensive coverage of the experiment at hand – in your own words. Only pertinent
articles or textbook materials relevant to the assigned experiment are cited. The underlying
physical principles, laws and governing equations relevant to the problem are presented in here.

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The literature may reveal conflicting views and opinions on the topic; these are included in the
review in an unbiased way. State the assumptions and limitations of the theory, if any. Charts,
diagrams, and other exhibits may be used in developing and explaining the theory, especially if
they aid clarity and conciseness.

4. Methodology
This section gives details of how the experiment is accomplished. This is a rewrite – in proper
tense, with any needed additions, corrections and improvements – of the Lab Proposal.
Assumption and justification involved while doing the experiment and preparing the report may also
include. Importance and information on precautious/safety aspect of the experiment may also be
highlighted and discussed, if any. This rewrite should now reflect the actual experimental work
done by your team, and thus be consistent with the upcoming results and discussion sections.

5. Results
The results section delivers the evidence that will help answer the questions raised by the objective
and scope of experiment, should prepare readers for the more detailed upcoming discussion, and
justify the conclusions that will be drawn later on.

Observations, data and calculated results (in consistent units) are often presented best as graphs
or charts, particularly if it will be important to illustrate trends. However, tables make sense when
you need to present accurate data and specific facts or demonstrate the relationships between
numerical and/or descriptive data. Figures and tables should include – whenever possible –
published, theoretical, and/or model/simulation values available from the literature or produced
programmatically. Tables of raw experimental data are not placed in this section; they are reported
in appendices. Other results that do not relate directly to the upcoming discussion should either
be reported in the appendices. Data are often summarized or reduced/condensed for presentation.
Reducing the data allows generalizations to be made and trends to be pointed out.

Obviously, then, charts and tables must be accompanied by appropriate text. Every figure or table
itself is numbered and supplied with a brief but descriptive title or caption. Build graphics and other
visual displays so that, with their accompanying text/description, they are self-explanatory. The
text must briefly explain how the results were obtained from the experimental data, the associated
quantitative uncertainty (e.g., confidence limits, standard error, etc. if necessary), references to
appropriate equations or sample calculations, and any critical assumptions or approximations
made in obtaining the results. However, best practice in bringing together your exhibits and your
words is accomplished by referring readers to graphics explicitly and telling them what trends to
notice.

6. Discussion
If the results section delivers the evidence, the discussion section makes the case in court. It must
answer and reflect to the objective and scope of experiment. In the discussion section, you explain
what your experimental results mean by relating them to the concepts and ideas presented in the
introduction and literature review/theory sections.

There are many questions that could be answered in this section so you should not limit yourself
to those offered here as examples. Answer the questions that make most sense for your work.

 Do the results agree with theory, with the work of others, with models/simulation? If so,
how? If not, why not? Can the disagreement be explained?
 What are the most probable sources of experimental error and have these affected your
ability to draw conclusions? How might these errors have been reduced or eliminated?
 Did your results reveal problems with the experimental plan, method, or equipment? How
might these be improved?

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 Were your assumptions suspect or reliable?

 What definite conclusions can you draw from your results? What conclusions are more
speculative?
 What implications do your results have on theory and/or current industrial practices?
 What questions remain unanswered? What questions should be answered next?

In this section, you may also criticize the lab experiment and make recommendations or
improvement. Such criticisms and recommendations, however, should focus on the lab as a
learning process; mere complaints about faulty equipment or amount of time spent are not
appropriate.

7. Conclusion
Draw conclusion from the results and discussion that answer the objective and scope of experiment.
Then go on to explain your conclusions that summarizes and reflects the results and discussion.

8. Nomenclature
All symbols and acronyms used in the report and its appendices must be listed and defined in a
nomenclature section with the consistent set of units used for calculation/reporting of results.
Symbols are arranged in alphabetical order, Latin terms (e.g., a, b, D, Re, Pr, etc.) first, followed by
Greek (e.g., α, β, ρ, etc.), and finally subscripts (e.g., i, j, k, etc.). Greek and subscript sets are
headed by the titles ‘Greek’ and ‘Subscripts’.

In addition to the nomenclature section, introduce these symbols where they first appear using
either running text or a list set off from the running text. If a dozen or fewer symbols are used in
this report, you may rely on the in-text introduction of symbols and acronyms alone and forego a
separate nomenclature section altogether.

9. References
The references section includes all references from which material in this report was taken. It does
not include materials consulted but not cited. It does include citations listed in any appendix
document (e.g., citing of handbooks from which properties data have been taken). A report without
ANY cited literature is typically not a credible piece of work. Citing the literature typically strengthens
any case you are making in your own reporting.

The in-text citations themselves should give the page number(s) relevant to the actual material
cited. The in-text citation plus the full reference in the references section make it possible for the
reader to find the material.

The referencing format should follow the one that is standard for UTM.

10. Appendices
Appendices may include raw data, calculations, graphs, and other quantitative materials that were
part of the experiment, but not reported in any of the above sections. Refer to each appendix at
the appropriate point (or points) in your report. For example, at the end of your results section, you
might have the note, See Appendix A: Raw Data Chart.

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EXPERIMENT 1: LIQUID-LIQUID EXTRACTION

OBJECTIVE OF EXPERIMENT

In this experiment, you will study the transition of a component from two-component liquid mixture
(feed) into a solvent by extraction.

SCOPE OF EXPERIMENT

1. To determine a mass fraction of ethanol via the density calculation.

DESCRIPTION OF A LIQUID-LIQUID EXTRACTION

Liquid-liquid extraction refers to the dissolving out of one or more components of a liquid mixture
using a solvent. Examples of liquid-liquid extraction are:
a) Separation of aromatic compounds from crude oil fractions.
b) Separation of vitamins from aqueous solutions.
c) Removal of lecithin from vegetable oil.

Therefore, liquid-liquid extraction involves at least three liquids. Names such as transition
component, carrier liquid and solvent as showed in Figure 1. The carrier liquid and solvent together
form a phase boundary. They are insoluble in one another. This is the condition so that separation
into two phases can occur after the actual extraction. Also required is a clear density difference
between the carrier liquid and solvent.

In Figure1, the solvent is specifically heavier than the carrier liquid. Therefore, the carrier liquid
floats on the solvent. The carrier liquid "carries" the transition component, the transition component
is dissolved in the carrier liquid. The next step shows is the mixing of the two liquid phases. Droplets
are formed, the specific surface area increases and the three liquids are brought into intensive
contact. In doing so, the transition component transfers from the carrier liquid into the solvent.
Another condition for extraction is that the transition component is soluble in the solvent. After
mixing, two further liquid phases form. The specifically heavier solvent settles downwards (settling).
The transition component is dissolved in the solvent. The carrier liquid floats. Finally, the two liquid
phases are transferred into separate beakers. In process engineering, we are often interested in
the incoming and outgoing materials and material flows. Figure 2 expands the graphical
representation from Figure 1 with the corresponding terms.

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Figure 1: Simplified representation of liquid-liquid extraction

Figure 2: Liquid-liquid extraction, identification of incoming and outgoing materials

The following terms are common in liquid-liquid extraction: The liquid mixture of the transition
component and carrier liquid is called the feed. The two liquid phases, which we get at the end of
liquid-liquid extraction are called the extract and the raffinate. The extract is essentially a solution
of the transition component in the original solvent. The raffinate is essentially the original feed, less
the extracted proportion of the transition component.

DESCRIPTION OF EXPERIMENT

Figure 3 shows the process diagram for the CE 620 liquid-liquid extraction unit. At the beginning of
extraction, solvent is located in the solvent tank. At the beginning of extraction, feed is located in
the feed tank. After extraction, extract is located in the solvent tank. After extraction, raffinate is
located in the feed tank. The mass transfer of liquid-liquid extraction takes place in the extraction
column K1. This is where feed and solvent meet. When this happens, a part of the transition
component is extracted from the feed into the solvent. The feed is continuously pumped from the
feed tank B5 by the feed pump P2 into the bottom of the extraction column (feed inflow). The feed

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moves upwards in the extraction column. From the top of the extraction column the feed returns to
the feed tank (feed return). The solvent is continuously pumped from the solvent tank B1 by the
solvent pump P1 into the top of the extraction column (solvent inflow). The solvent moves
downwards in counter flow to the feed. From the bottom of the extraction column, the solvent returns
to the solvent tank (solvent return). The driving force for the counter flow is the density difference
between solvent and feed. Therefore, the material and/or the mixture with the lower density must
be pumped into the bottom of the extraction column.

Figure 3: Process diagram of the CE 620 liquid-liquid extraction system

GENERAL START-UP PROCEDURES

1. Make sure all valves are closed

2. Remove cover from tanks B1 and B3-B5
3. Connect trainer to the mains power supply
4. Turn main switch

EXPERIMENTAL PROCEDURE

The following chemicals will be used in the experiment

1. Ethanol (transition component-feed)

2. Cooking oil (carrier liquid-feed)

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3. Water (solvent)

The experimental conditions are

1. Extraction of ethanol from cooking oil with water

2. Mass fraction of ethanol in the feed 10%
3. Equal masses of feed and solvent, each 3L
4. Extraction time 60 min
5. Solvent flow 24 L/hr
6. Feed flow 48 L/hr

Steps to fill feed and solvent into tank B5 and B1 respectively

1. Pour feed into feed tank B5. Ethanol should be added first!
2. Stir feed for 10 minute
3. Pour solvent into solvent tank B1

Conducting the liquid-liquid extraction experiment (batch)

1. Ensure that valve V30 is opened

2. Fully open regulating valve V4 for feed return
3. Close regulating valve V3 for solvent return
4. Start solvent pump P1
5. Using regulating valve V1, adjust solvent flow to about 4.8 L/hr
6. Start feed pump P2.
7. Using regulating valve V2, set feed flow to about 48 L/hr
8. Watch as the extraction column K1 fills up
This is the start of extraction

9. Start stopwatch. Get a sample of extraction from solvent tank B1 for density measurement
(at the start of extraction)
10. Using regulating valve V1, increase solvent flow to about 24 L/hr
11. Open regulating valve V3 for solvent return about one turn
12. Check that the feed flow is about 48 L/hr. Readjust with V2 if it is different.
13. At regular intervals, for example after every 10 minutes, get the sample from solvent tank
B1 and measure the density measurement and temperature as tabulated in Table 1. From
the density value, find the mass of ethanol fraction based on the provided Calibration table

Caution!
Make sure the phase boundary is at 50% throughout the extraction process. If the
phase boundary deviates significantly from half the extraction height, adapt the
opening of regulating valve V3 for solvent return:
– If the phase boundary is falling, close regulating valve V3 a little more
– If the phase boundary is rising, open regulating valve V3 a little more

14. After 60 minutes of extraction time, stop pumps P1 and P2

This is the end of extraction

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Conducting the density measurement

1. The density measurement is carried out using a volumetric flask (100mL)

2. Pour a sample of just over 100mL of liquid into a beaker
3. Use a hand-held thermometer to determine the temperature of the sample and note it down
4. Place clean, dry volumetric flask on the analytical balance
5. Tare analytical balance
6. Take the volumetric flask in one hand and the beaker in the other
7. Pour liquid mixture into the volumetric flask to about 100 mL
8. Place volumetric flask back on the analytical balance
Use the pipette to add sample into the volumetric flask, until it reaches 100mL
Read mass of the tare and note it down based on Table 1

Cleaning the beaker and volumetric flask every time you take a new sample

GENERAL SHUT-DOWN PROCEDURES

1. Close regulating valves V1- V4

2. Open valve V30
3. Now the oil phase settles on the water phase
4. By opening the regulating valve V3, the solvent from the extraction column can flow back into
solvent tank B1
5. Close V3 as soon as the phase boundary reaches the base of the extraction column
6. By opening valve V28, pour feed from the extraction column into the measuring beaker
7. Then, by opening valve V29, the remaining feed can flow from the extraction column into the
measuring beaker
9. Drain measuring beaker into the feed tank B5.

RESULTS & DISCUSSION

1. Why ethanol should be added first before cooking oil. Discuss the fundamental of that
procedure.

2. Table 1: Worksheet of standard liquid-liquid extraction experiment, batch mode.

Measurement Evaluation Notes

Δtextraction Temperature Density Mass fraction of
(min) (oC) (g/100mL) ethanol , WE (TX), %
0
10
20
30
40
50
60

Manual Prepared by:

Norhuda binti Abdul Manaf

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EXPERIMENT 2: DISTILLATION
OBJECTIVE OF EXPERIMENT

In this experiment, you will study the effect of reflux ratio to density of the feeding mixture,
residues, and distillate in distillation unit.

SCOPE OF EXPERIMENT

1. To investigate the effect of reflux ratio to the density on the feeding mixture, residues, and
distillate.

DESCRIPTION OF EXPERIMENT

Distillation is a process including heat and material transfers in order to separate one or several
products of relative different volatility. The separation is carried out by a chaining of vaporizations
and condensations. Based on volatility differences, the heat causes components with lower
boiling points to be vaporized, leaving less volatile components as liquids. It is collected as
distillate with high purity. Distillation can be used to separate binary or multi-component mixtures.
Vapor produced from a mixture is in equilibrium with the mixture is in equilibrium with the mixture
phase which has a higher composition in the most volatile compound.

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SCHEMATIC DIAGRAM OF THE PILOT PLANT SETUP

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EXPERIMENTAL PROCEDURE

The objective of this experiment is to investigate the influence of reflux ratio on the feeding mixture,
residues, and distillate. There are several parts of work involved as follows:

Part 1: Loading the feed mixture into the feed tank (TK1)

1. Mix in 3 liter of ethanol and 4 liters of tap water.

2. Fill in TK1 with the mixture.
3. Connect the silicone flexible on the draining valves of the distillate and bottoms products tank
(TK2, TK3).
4. Make sure of the silicone flexible put into the cap.
Part 2: Activating the control panel

1. Turn clockwise the MAIN SWITCH at the control box to ON the unit.
2. Check the emergency stop button is freed by turning the key (Please let the emergency key
as it is).
3. When the power is supplied to the unit, the power indicator will turn to white.
4. Switch ON the GENERAL ON switch. The green light means that power supply is available
for each actuator.

Part 3: Loading of the reboiler by feed pump (P1)

1. Ensure V4, V7, V10, V9, and V2 is closed before turning on the P1.
2. Open the valve V1.
3. Put the 3 ways valve V5 in position to fill up the reboiler (3 o’clock position).
4. Put the 3 ways valve V6 in position to use the thermal siphon re-boiler (12 o’clock position).
5. Make sure that the outlet flexible tubing of feed pump P1 is filled with liquid mixture.
6. Activate the feed pump P1 by turning on the P1 General On switch.
7. Open the valve V3.
8. Loading the reboiler up to overflow line.
9. Set up the feed flow rate to 20 L/h by adjusting the FI4.

Part 4: Water feeding of condenser and refrigerants

1. Open valve V19.

2. Open valve V20 and set up flow rate at 60 L/h.
3. After the cooling water circulating inside the distillation unit, then start the heating.

Part 5: Heating

1. Ensure the cooling water is circulating in the distillation unit before start the heating.
2. Switch ON the electrical heater on the control box.
3. On the touch screen, adjust the boiler percentage to 50 %.
4. Observe vapours coming up into the distillation column.
5. Put valve V5 in position, such that the mixture flows into the middle of the distillation column
when the mixture is boiling.
6. Observe the column pressure drop, the normal value is 100 mm of water.
7. Adjust the boiler percentage (power) based on pressure inside the boiler.
8. Observe the vapors condensed in the condenser.
9. If the pressure is too high (more than 100mm), reduce the boiler percentage and the charge
pump flow rate.

Part 6: Reflux ratio adjustment

Working principle:
L
R
The reflux ratio R definition in this experiment is D
L: Part of the liquid flowing back to the column (FI1 flow rate)

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D: Part of the liquid drawn off (production) (FI2)

Regulate these flowrates to adjust the reflux ratio.

1. Ensure the vapor condenses and fills up condenser ECH3.

2. Open up reflux flow valve, V12 and distillate flow valve, V13.
3. Switch ON the pump P2.
4. Ensure there is no air bubble inside the flow meter.
5. Adjust valves V12 and V13 to the reflux ratio of 0.5 (2.0 for next experiment).
6. Wait until the system is stable.
7. After the system is stable, collect the 100 ml of mixture from cooled residue opening, V8,
cooled distillate opening, V10 and feeding mixture opening, V4. Open slightly and slowly the
valve less than 45 º. To take the samples of the mixtures in the equilibrium into the column, it
is important to open the valve very slowly so that, there are no creation of depression at the
level of the valve and break the column equilibrium.
8. After collected the mixtures from each reflux ratio, open V17 and V16 to drain the ethanol and
water in the TK1.
9. Measure the density of each samples from each reflux ratio.
10. Record and write down the results in the table.

Part 7: Residue extraction

1. Switch ON P3 from control box.

2. Open the valve V8.
3. Adjust the extraction flow from valve V11 to maintain a constant level into the reboiler.
4. The liquid flow into the reboiler must be maintained as constant as possible.

Part 8: Stop at the end of the workshop

1. Stop all the pumps and the boiler heating.

2. Keep the cold water circulation flow rate of 200 L/h into the condenser.
3. Wait for the boiler to cool down at least 30 ºC on TI1 indicator.
4. Clean the unit and experimental area.
5. Power off the electric control box with the main switch. Lock the main switch.
6. Close all the valve.

RESULTS & DISCUSSION

1.0 Complete the following table:

Conditions: 0.5 reflux ratio
FI1 FI2 Reflux ratio

Density Mass fraction of ethanol , W E (TX), %

V8 V10 V4 V8 V10 V4

Temperature (after weighing) Temperature inside system

V8 V10 V4 V8 V10 V4

Conditions: 2.0 reflux ratio

FI1 FI2 Reflux ratio

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Density Mass fraction of ethanol , W E (TX), %

V8 V10 V4 V8 V10 V4

Temperature (after weighing) Temperature inside system

V8 V10 V4 V8 V10 V4

2.0 Plot:
i) The graph mixture density versus reflux ratio.
ii) The graph mass fraction of ethanol versus reflux ratio.

3.0 Based on the calibration tables (Appendix 1), deduce the mass fraction of ethanol and other
compositions inside the sample.

4.0 Determine the optimum reflux ratio based on the graph.

5.0 Describe the difference in measuring the density between the method that been used in this
experiments and other methods.

6.0 Explain and describe the heating principle in this continuous distillation unit.

7.0 Draw the mechanism of continuous distillation systems that used in this experiment and explain it.

8.0 Identify and describe the factors that affecting distillation column operation.

9.0 Identify and describe each valves and parts purpose.

Manual Prepared by:

M. P Khairunnisa

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EXPERIMENT 3: EVAPORATION

OBJECTIVE OF EXPERIMENT

In this experiment, you will study the efficiency of a double effect evaporator

SCOPE OF EXPERIMENT

2. To determine calculate the concentration of the solutions at different stages of double effect
evaporator
3. To determine the efficiency and the energy consumption of the double effect evaporator

DESCRIPTION OF DOUBLE EFFECT EVAPORATOR

Evaporation is a method for concentrate a solution containing non-volatile solute and volatile solvent
(or a relative higher volatility solute). Evaporation is commonly used process in industries, such as
pharmaceutical, chemical, food processing, cosmetics and perfumes. Evaporation process enables
solvent to be regenerated and reused in extraction process.

DESCRIPTION OF EXPERIMENT

The double effect evaporator has 4 major flows in the equipment, which include sample solution,
steam, cooling water and vacuum.

The sample solution flows from sample tank R1 into Evaporator 1 (EVP1) and it is associated phase
separator (cyclone – C1). The liquid phase product of C1 partially returns into EVP1 and the rest are
directed into Evaporator 2 (EVP2) for further separation. The vapor phase product from C1 heats the
sample solution in EVP2. Then, the vaporized sample in EVP2 flows into Cyclone 2 (C2). The liquid
product of C2 collected as the concentrated solution in R2, while some of the liquid returns into EVP2.
The vapor product of C2 condenses through condenser ECH1 and keep in tank R3.

Steam supply is generated by the steam generator. The steam supplies to the EVP1 for heating and
evaporating the sample solution. Tap water supply is used as cooling water of the system. The water
supplies to steam generator, Liebig’s condenser (bottom of evaporator) and condenser ECH1. The
vacuum system provides vacuum condition in the EVP2, which reduces the boiling point of the sample
solution in EVP2.

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Figure 1.1: Schematic diagram for the double effect evaporator

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EXPERIMENTAL PROCEDURE

The objective of this experiment is to determine the evaporation efficiency of the equipment. The
procedure for this experiment is listed as following:

1. Start steam generator

i. Close valves 17 and 18.
ii. Switch on steam generator power supply.
2. Prepare sample solution
i. Dilute 1.5kg of sugar in 15L of deminerised water.
ii. Stir solution in feed tank R1.
iii. Take sample from R1 and check reflective index of the sample using reflectometer.
3. Start equipment
i. Ensure that R2 and R3 are clean.
ii. Switch on power supply.
4. Start cooling system
i. Open water supply to the equipment.
ii. Open valve V14 and V15 and set water flow rate (F11) in the condenser at 200 L/h.
iii. Open valve V16 slightly and to allow cold water into the Liebigs condenser.
5. Supply solution to the evaporator
i. Put suction tube of feed pump P1 in the feed tank R1.
ii. Switch on pump P1 on the control panel and set struck power to 70%.
iii. Open valve V1 and measure filling rate.
iv. Fill evaporators until the level of EVP1 reach level LL1 and half of EVP2, through the
evaporator draining mode into ‘forced’ on control panel.
6. Regulate process pressure
i. Switch on vacuum pump on control panel.
ii. Close valve V11 and V13.
iii. Create a slight leak using valve V11 to stabilize the pressure at (less than) 500 mbar abs.
7. Feed steam to the evaporators
i. Turn the evaporators draining mode into ‘auto’ on control panel.
ii. Open valve V18 and slowly open valve V17.
iii. Set the steam pressure on the nanometre PI1 at 0.5 bar relative via V15.
8. Wait until the operating condition stable (about 15 minutes)
9. Start stopwatch and record experiment data according to the data sheet given
10. At the end of the experiment,
i. Close valve V17 and V18 for the steam feed with heat resistance gloves.
ii. Switch off steam generator.
iii. Switch on feed pump P1 on the control panel.
iv. Switch off vacuum pump on the control panel.
v. Empty R2 and R3 into beakers using V8 and V10.
vi. Weight the solution collected from R2 and R3 as well as the remaining solution in tank
R1.
vii. Take sample from each solution to determine concentration using reflectometer.
11. Clean the equipment after all samples and measurements taken.
i. Replace solution in tank R1 with clean water.
ii. Switch off feed pump P1 on the control panel
iii. Switch off vacuum pump on the control panel.
12. Shutdown the equipment when TI2 and TI3 are less than 60 ⁰C
i. Switch off feed pump P1 on the control panel.
ii. Switch off vacuum pump on the control panel.
iii. Open valves V11 and V13 to bring the process back to atmospheric pressure.
iv. Close valve V14, V15, and V16 for the cooling circuit of condenser and Liebig.
13. Empty the equipment by opening different valves available at each part of the equipment.

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RESULTS & DISCUSSION

1. Complete the following table for the calibration of the quantification for the sugar aqueous
solution

Sugar concentration in 100g water Refractive index

(g)
0
10
20
30
40
50
60

2. Record all data required in the experiment datasheet.

4. Calculate the efficiency of the double-effect evaporator.

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Experiment Data

Parameter for evaporation:

Pressure of the heating steam: bars relative

Feed flow rate (stoke power): %
Feed flow rate: mL/min
Cold water flow rate: L/h
Reduced pressure for EVP2: mbars abs

Volume of Volume of
Time Temperature (°C) concentrated evaporated
(mins) solution, R2 solution,
T1 T2 T3 T4 T5 T6 (L) R3 (L)

Feed solution: Initial weight g Final weight:

g
Concentrated solution: Final weight: g Refractive index:
Evaporated solution EVP1: Final weight: g Refractive index:
Evaporated solution EVP2: Final weight: g Refractive index:

Manual Prepared by:

Liew Peng Yen

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EXPERIMENT 4: GAS LIQUID ABSORPTION

OBJECTIVE OF EXPERIMENT

In this experiment, you will study the absorption of carbon dioxide from air using sodium
hydroxide.

SCOPE OF EXPERIMENT

1. To operate gas-liquid absorption process using packed column gas absorption unit
2. To analyze the sample using direct titration method to determine the amount of unreacted
NaOH in the sample.

DESCRIPTION OF EXPERIMENT

Absorption is an operation of separation which involves the transfer of a gas solution towards an
absorbing liquid having a weak volatility. This transfer is the result of the preferential dissolution of
the solute in the liquid phase. Desorption is inverse process and the volatile gas dissolved in
liquid phase is transferred in the gas phase. This transfer is favoured with the heater of this liquid
or with the stripping of a sluggish gas constituents.

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SCHEMATIC DIAGRAM OF THE PILOT PLANT SETUP

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EXPERIMENTAL PROCEDURE

CAUTION: Please carry out this experiment with proper personal protective equipment
(PPE). Ensure face mask, safety gloves and goggles are worn all the time when carrying out
these activities.

Part 1: Pre-experiment setup

1. Prepare 10L of 1M Sodium Hydroxide and put it inside the feeding tank.
2. Prepare 1L of 0.5M HCl for titration.
3. Carry out titration with both Sodium Hydroxide solution (refer Part 3).

Part 2: Start-Up
1. Ensure that all valves are closed.
2. Connect the air compressor to the port.
3. Start the pump and adjust the flowrate to 10L/h.
4. Fill the column until it starts to overflow.
5. Turn on the compressed air and adjust the flowrate to 1000 L/h (float height 60mm).
6. Start the stopwatch.

Part 3: Sample Collection

1. At t = 10 min, collect sample from V12.
2. Dilute about 10 mL of the sample in 100 mL of water.
3. Add a few drops of phenolphthalein.
4. Titrate 0.5M HCl into the mixture until change in colour (pink to colourless). Record the
volume as V1.
5. Add a few drops of methyl orange into the solution.
6. Titrate 0.5M HCl into the mixture until there is colour change (orange to pink). Record the
volume as V2.
7. Carry out sampling at every 10 minutes’ interval for 60 minutes.

Part 4: Shut Down

1. Turn off the gas valve and power switch for compressed air.
2. Turn off the pump. Close off V2 and V3.
3. Open V5 to drain the column. Close the valve.
4. Open V13 and V11 to drain the receiver and the bubbling pot. Close the valve once empty.
5. Open V4 to drain the gas mixture pipe. Close the valve once empty.
6. Open V1 to drain the anti-pulse tank. Close the valve once empty.

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RESULTS & DISCUSSION

1.0 Complete the following table:

Table 1: Titration values for samples from column (V12)
Time (Min) Initial 10 20 30 40 50 60
V1
V2
∆V

2. Calculate the percentage of CO2 removed at every interval.

3. From the data obtained, plot the operating line of the absorber. (Take y=x as equilibrium line)
4. Use the obtained data to calculate the packing height.
5. Compare the obtained packing height with the actual packing height

Theory
The reaction between sodium hydroxide and carbon dioxide will produce water and sodium
carbonate:
2 𝑁𝑎𝑂𝐻 + 𝐶𝑂2 → 𝑁𝑎2 𝐶𝑂3 + 𝐻2 𝑂
For the 1st equivalence titration (with phenolphthalein), the reaction is as follows:
𝐶𝑂3 2− + 𝐻 + → 𝐻𝐶𝑂3 −
𝑂𝐻 − + 𝐻 + → 𝐻2 𝑂
While for the 2nd equivalence titration (with methyl orange), the reaction is as follows:
𝐻 + + 𝐻𝐶𝑂3 − → 𝐻2 𝐶𝑂3
Sample calculations
Table 2: Titration values of V6 sample at 40 minutes
Time (Min) 40
V1 20.00
V2 20.02
∆V 0.02

Since ∆V= 0.02 mL means there is 0.02 mL of HCl reacted with sodium carbonate in the 10 mL
sample.

20 – 0.02 = 19.98 mL of acid reacted with excess sodium hydroxide, meaning:

0.5 × 19.98
[𝑁𝑎𝑂𝐻] = = 0.999 𝑀
10

Initial concentration of NaOH is 1M at 10L/h flowrate

Therefore, (1 − 0.999) × 10 = 0.001 mol of NaOH have reacted with CO2 in the column
From Equation (1), we know that 2 mol of NaOH reacted with 1 mol of CO 2

Therefore 0.001/2 = 0.0005 mol/h of CO2 reacted in the column.

CO2 constitutes 0.03% of air volume, therefore at 1000L/h of air,

0.03
× 1000 = 0.3 L/h of CO2
100

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Assume reaction at room temperature and condition,

0.3
= 0.0125 mol/h of CO2 at inlet.
24

0.0125−0.0005
Therefore, percentage of CO2 removal = × 100% = 96% CO2 removal
0.0125

2. Column Efficiency & Packing height Calculation

Column efficiency can be measured using Height Equivalent to Theoretical Plate (HETP)
Given that packing height,
𝑧 = 𝐻𝐸𝑇𝑃 × 𝑁𝑡
Where 𝑁𝑡 = Number of theoretical stages, which can be calculated using formula,
𝐴
𝑁𝑡 = 𝑁𝑂𝐺 ln(1⁄𝐴)
1−𝐴
Where NOG = Number of gas transfer units

Manual Prepared by:

M. P. Khairunnisa
Muhammad Syafiq Ridhwan Bin Mohd Nasir

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EXPERIMENT 5: OPEN ENDED – SHORT PATH DISTILLATION

MEMORANDUM

Dear students,
A new short path distillation unit has been completely assembled and
commissioned in Unit Operation Lab and ready to be used. Short path distillation
is a continuous separation process working under vacuum conditions. As a
chemical engineer to be, you are required to conduct an experiment using this unit
which can relate to the thermal separation process for thermal sensitive products.
Typical applications are high molecular organic compounds particularly form the
field of chemistry, pharmaceutical and food industry.
As an initial stage, you are required to prepare a proposal on the efficiency of
ethylene glycol – water separation in a short path distillation unit by manipulating
either stirrer speed or evaporator temperature. You are given one week to produce
a proposal and another one week to evaluate your finding. As this is your first
experience in handling the process/unit, you may need to discuss the
fundamental/literature review of short path distillation that used for thermal
separation under vacuum condition. At the same time, you need to investigate the
instrument setting, namely evaporator temperature, vacuum pressure, feed flow
rate, stirrer speed and contact time.
For your information, the operation of this unit will involve with high temperature
and vacuum pressure, thus SAFETY PRECAUTION should be listed out in the
proposal (including start up, shut down, cleaning) before you come out with the
experimental procedure. Additionally, you may need to select few parameters
(temperature, stirrer speed and etc.) and its best operating conditions that can help
to improve efficiency of the process. The selected parameters and operating
conditions should be justified with the experimental analyses. Figure 1 illustrates
schematic diagram of the unit to help you conducting the experiment.

Good luck!
Thanks.

Lab Coordinator

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Figure 1: Schematic diagram of short path distillation unit

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APPENDICES

Appendix 1: h, x graph for humid air

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Appendix 2: Ethanol/water mixture: Density in kg/m3 as a function of mass fraction of ethanol wE

and temperature T, 0 %≤wE≤50 %, 20 °C≤T≤30 °C

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Appendix 3: Air Flow Meter Data

SMJC 3731 CHEMICAL PROCESS ENGINEERING LABORATORY 3