LABORATORY REPORT

CHEMICAL ENGINEERING LABORATORY V (EP 212)

NUMBER OF EXPERIMENT: 7

EXPERIMENT TITLE: BATCH DISTILLATION AT CONSTANT REFLUX

LAB SESSION/GROUP NUMBER: THURSDAY

STUDENT NAME: LORNA AHLAAMI BT RAMZAN

STUDENT ID: 1001851777

TUTOR’S NAME: MS YING TAO CHUNG

DATE OF EXPERIMENT :2/7/2020 DATE OF SUBMISSION :9/7/2020

FACULTY OF ENGINEERING
PROBLEM STATEMENT:

Batch distillation has regained it interest from industries recent years. This is mainly
due to its flexibility and capability to produce high purity product. This interest has drawn
many researcher attentions to invent a fast and reliable model to serve the industry. To date,
several type of simulation model had been presented, and the interest to obtain a better control
and improvement on batch distillation has yet to stop. In this experiment, the problem is to
examine the change in top and bottom composition over time in batch distillation. The
compositions obtained from the experiment were determined using Refractive Index method.

HYPOTHESIS:

The experiment conduct the batch distillation at constant reflux to examine the change in top
and bottom composition.

OBJECTIVES:
● To operate a batch distillation unit at constant reflux
● To examine the change in top and bottom composition over time in batch distillation
● To measure the refractive index of samples using a refractometer

INTRODUCTION:

When there are differences in volatility of components in a boiling liquid mixture

distillation is the best way to separate the substances. ‘Batch’ distillation refers to the use of
distillation in batches, it has a tank with the mixture to be separated and then mixture is to be
heated to produce vapor. The vapor leaves the tank and passes through the column where the
separation takes place. At the top of the column, the vapor is condensed and part of the liquid
produced flows down the column in the counter current flow with the vapor rising up the
column. The other part of the condensate is drawn off as the overhead product and the
remaining at the bottom column is the bottom product.
 If small quantities of material at regularly scheduled periods are used, then batch distillation
is preferred over continuous distillation. The main steps in the batch distillation are operated
discontinuously. In contrast with a continuous process, batch processes deliver the product in
discrete manner. Reflux in distillation refers to the return of a portion of condensed distillate
back to the reaction vessel. The advantage of this technique is that it can be left for a long
period of time without the need to add more solvent or fear of the reaction vessel boiling dry
as any vapor is immediately condensed in the condenser. For batch distillation at constant
reflux ratio, R is kept constant and distillation is continued until the distillate composition
dropped below a certain pre-specified level.

MATERIAL AND APPARATUS

Batch distillation unit, refractometer
PROCEDURES

1. The general start-up procedures were performed.

2. The power heater was set to 2.0 kW and the reboiler temperature were allowed to reach
approximate 85 °C.
3. The reflux control was set to position 3.
4. The temperature when the top column temperature sensor TT 112 reached steady state
was recorded.
5. The sampling valve V9 was opened and 100 mL of distillate sample was collected using
a conical flask. The valve V9 was then closed.
6. The bottom overflow level was adjusted. Valves V2 and V3 were opened and 100 mL
of sample bottom product was collected using a conical flask. The valves V2 and V3
were then closed.
7. The refractive index of the samples were measured and the values were recorded into
the data table.
8. Steps 4 to 7 were repeated until the bottom sample R1 values became constant.
9. The heater power was switched off and the system was allowed to cool down to ambient
temperature.
RESULTS AND QUESTIONS
Table 1: Composition Data Based on Refractive Index
Moles of
Mass of Mass of Moles of
Volume of Volume of Water Refractive
Ethanol Water Ethanol
Ethanol (ml) Water (ml) (mol) x Index
(g) (g) (mol) x(10-2)
(10-1)

0 10 0 10 0 5.5494 1.333
1 9 0.789 9 1.7126 4.9945 1.338
2 8 1.578 8 3.4252 4.4395 1.342
3 7 2.367 7 5.1378 3.8846 1.349
4 6 3.156 6 6.8505 3.3296 1.350
5 5 3.945 5 8.5631 2.7747 1.353
6 4 4.734 4 10.276 2.2198 1.353
7 3 5.523 3 11.9883 1.6648 1.355
8 2 6.312 2 13.7009 1.1099 1.357
9 1 7.101 1 15.4135 0.5549 1.360
10 0 7.89 0 17.1261 0 1.361

Table 2: Mole fraction of ethanol based on Refractive Index

Time distillate Bottom
Refractive Mole fraction Refractive Mole fraction
index ethanol (10-2) index ethanol (10-2)
mol mol
10 1.3502 6.9646 1.3512 7.53554
20 1.3560 12.8446 1.3491 5.30907
30 1.3602 15.7560 1.3423 3.4986
40 1.3605 16.2698 1.3351 0.7193
50 1.3609 16.9548 1.3351 0.7193
 Refractive index vs mol fraction of ethanol

To calculate mol fraction of ethanol at table 2. Use linear interpolation

𝒚 − 𝒚𝟏 𝒙 − 𝒙𝟏
=
𝒚𝟐 − 𝒚𝟏 𝒙𝟐 − 𝒙𝟏

𝟏. 𝟑𝟓𝟎𝟐 − 𝟏. 𝟑𝟓𝟎 𝒙 − 𝟔. 𝟖𝟓𝟎𝟓

=
𝟏. 𝟑𝟓𝟑 − 𝟏. 𝟑𝟓𝟎 𝟖. 𝟓𝟔𝟑𝟏 − 𝟔. 𝟖𝟓𝟎𝟓

X= 6.9646 10-2 mol

2) USING X-Y EQUILIBRIUM DIAGRAM FOR ETHANOLWATER SYSTEM, MARK

THE TOP AND BOTTOM COMPOSITION FOR EACH SAMPLING TIME ON THE
DIAGRAM. OBSERVE THE CHANGE OF COMPOSITION OVER TIME IN THE BATCH
DISTILLATION COLUMN.

3) PLOT GRAPH OF COMPOSITION VS TIME

 10 min Equilibrium Diagram for Ethanol-Water System at 1 atm
1

0.9

0.8

0.7
Vapor mol fraction

0.6

0.5

0.4

0.3

0.2

0.1

0
Xd Xb
0 0.2 0.4 0.6 0.8 1
Liquid mol fraction

20 min Equilibrium Diagram for Ethanol-Water System at 1 atm

1

0.9

0.8

0.7
Vapor mol fraction

0.6

0.5

0.4

0.3

0.2

0.1

0 Xb Xd
0 0.2 0.4 0.6 0.8 1
Liquid mol fraction
 30 min Equilibrium Diagram for Ethanol-Water System at 1 atm
1

0.9

0.8

0.7
Vapor mol fraction

0.6

0.5

0.4

0.3

0.2

0.1

0
Xb Xd
0 0.2 0.4 0.6 0.8 1
Liquid mol fraction

40 min Equilibrium Diagram for Ethanol-Water System at 1 atm

1

0.9

0.8

0.7
Vapor mol fraction

0.6

0.5

0.4

0.3

0.2

0.1

0
Xb Xd
0 0.2 0.4 0.6 0.8 1
Liquid mol fraction
 40 min Equilibrium Diagram for Ethanol-Water System at 1 atm
1

0.9

0.8

0.7
Vapor mol fraction

0.6

0.5

0.4

0.3

0.2

0.1

0
Xb Xd
0 0.2 0.4 0.6 0.8 1
Liquid mol fraction

Table 3 : Results of composition

Time 𝟏
Distillate composition , y Bottom composition, x
(min) 𝒚−𝒙
10 0.0696 0.0754 -172.4138
20 0.1284 0.0531 13.2802
30 0.1575 0.0350 8.1633
40 0.1627 0.0072 6.4309
50 0.1695 0.0072 6.1614
 Graph 1: composition vs time

DISCUSSIONS

Batch distillation column can be operated with three reflux policies in order to meet certain
product specification. The reflux policies that can be employed to a batch distillation are either
constant reflux, regulating reflux or optimum reflux.

In this experiment, the aim was to studied constant reflux. For constant reflux, distillate purity
for lighter component will drop over time. In order to maintained the purity of distillate over
time, regulating reflux policy can be employed. Optimum reflux policy is used when maximum
profit from the operation is required; it is a tradeoff policy between constant reflux and
regulating reflux policies.

Batch distillation with constant reflux ratio can be done by using Rayleigh equation in
conjunction with McCabe-Thiele graphical method. Batch distillation under constant reflux
can be analyzed mathematically by considering that the mole lost from the still represent moles
of distillate collected. The purpose of measuring the refractive index is to determine the
composition of samples collected.

The relationship of bottoms composition, Xb and distillate composition, xD is determined by

the assumption of refractive index made from table 2, and followed by mccabe thiele diagram
for stepping. Stepping from point Xd then connect to vapor mol of ethanol line then connect to
liquid mol ethanol line.

For the composition vs time graph, the composition were calculated by using
1
𝑚𝑜𝑙 𝑑𝑖𝑠𝑡𝑖𝑙𝑙𝑎𝑡𝑒 − 𝑚𝑜𝑙 𝑏𝑜𝑡𝑡𝑜𝑚

LIMITATION AND ERRORS OF THE EXPERIMENT

Throughout the experiment, some possible error can be identified. The refractive index
must be measured when the samples are completely cooled down. The position of eye should
be directly perpendicular to the scale of measuring cylinder. Record several temperature and
calculate the average temperature.

There are some precaution need to be aware before conduct the experiment. Wear a
safety glove when taking the samples out of the valves to avoid scalding. The distillate and the
bottom product can be hot as it is heated at 80 degree Celsius. It is advised be careful when
handling ethanol as it is highly flammable.
CONCLUSION

In constant reflux condition, the change in the overhead and bottom composition over
time in a batch distillation unit is determined. Theoretically, the mole fraction of ethanol in
both the distillate and bottom product decreases over time. As time elapse, the mole fraction of
ethanol in the evaporator decreases. At constant reflux, the amount of moles left in the
evaporator at any time can be determined. The objectives of this experiment are all achieved.

REFERENCES

1. Ms. Rafizah bt. Zaiton / Dr. Chung Ying Tao (2020). CHEMICAL ENGINEERING
LABORATORY 5 (EP212) LABORATORY MANUAL.

2. McGabe, Smith & Harriot, “Unit Operations of Chemical Engineering”, McGraw

Hill, (Singapore), 2001.

3. Geankoplis C.J., “Transport Processes and Unit Operations”, Prentice Hall,

(Singapore), 1995.
 FACULTY OF ENGINEERING
DEPARTMENT OF CHEMICAL & PETROLEUM ENGINEERING
LAB REPORT ASSESSMENT
Student Name: _________________________________________ Student ID: _____________

CLO / PLO Indicator Criteria Unacceptable Satisfactory Moderate Good Excellent Percentage Score
(0%) (25%) (50%) (75%) (100%) (%)
CLO1/PLO2 Creates Problem No problem Problem Problem statement Problem Problem 5
problem statement statement and statement and and objective miss at statement and statement and
statement and objective objective objective are least one important objective are objective are
including stated irrelevant or not consideration listed, important fully addressed
approximations appropriate to experiment
and the experiment details are
assumptions covered, some
minor details
missing
CLO1/PLO2 Identifies Experimental No procedures Procedures do Procedures are Procedures are Procedure are 5
known and procedures are written in not properly listed, but missing listed in listed in clear
unknown the report. demonstrate information. Known complete, steps. Known
information, the steps taken and unknown known and and unknown
uncertainties in the information, unknown information,
and/or biases experiment. uncertainties and information, uncertainties
biases are not listed. uncertainties and biases are
and biases all listed.
some are not
listed. But some
minor details
are missing.
CLO1/PLO2 Evaluates Discussion/ Incomplete Incomplete / Some of the results Almost all of the Important 10
results Observation and incorrect incorrect have been correctly results have trends and data
interpretation interpretation of interpreted and been correctly comparisons

Revised Jan 2019

 of trends and trends and discussed; Partial but interpreted and have been
comparison of comparison of incomplete discussed; only interpreted
data indicating data. understanding of minor correctly and
a lack of results is still evident. improvements discussed;
understanding are needed. good
of the results. understanding
of results is
conveyed.

CLO2/PLO4 Generates Hypotheses No Hypotheses is Hypotheses does not Hypotheses Hypotheses 10

working hypotheses is stated but involve parameters involve involve
hypotheses stated irrelevant the parameters but parameters and
experiment does not justify justify the
the relationships relationships

CLO2/PLO4 Assesses Conclusion No judgement Incomplete Data is validated. Data is Data is 10

validity of on data data on validity Only one of the validated. Only validated. All of
conclusions validity in the in the following is two of the the following
within conclusion conclusion assessed: following are are assessed:
limitations of 1. limitation assessed: 1. limitation
data and 2. experiment SOP 1. limitation 2. experiment
methodologies 3. experimental error 2. experiment SOP
SOP 3. experimental
3. experimental error
error
CLO2/PLO4 Synthesizes Conclusion Incorrect Incomplete Conclusion are Conclusion are Conclusion are 10
data to reach conclusion. conclusions. drawn. Only two of drawn. Only drawn. All the
conclusions Only one of the the following are three of the following are
following is addressed: following are addressed:
addressed: 1. results addressed: 1. results
1. results 2. discussion 1. results 2. discussion
2. discussion 3. hypotheses 2. discussion 3. hypotheses
3. hypotheses 4. objectives 3. hypotheses 4. objectives
4. objectives 4. objectives
CLO3/PLO10 Creates Results: No figures, Figures, Most figures, graphs, All figures, All figures, 10
figures, tables Data, figures, graphs, tables graphs, tables tables OK, some still graphs, tables graphs, tables

Revised Jan 2019

 and drawings graphs, are provided. contain errors missing some are correctly are correctly
to engineering tables, etc. or are poorly important or required drawn, but drawn, are
report constructed, features. some have numbered and
standards have missing minor problems contain
titles, captions or could still be titles/captions.
or numbers, improved.
units missing or
incorrect, etc.

CLO3/PLO10 Writes Appearance Appearance Sections out of Sections in order; Lab report is Lab report is 10
documents and and formatting order, report is Formatting is rough mostly typed / typed / written
using formatting totally not typed / but readable. written using the in well
engineering inappropriate. written using Appropriate formatted, very
report the appropriate format, all readable.
standards format. sections in
order,
formatting
generally good
but could still be
improved.

CLO3/PLO10 Delivers clear Spelling, Grammar / Frequent Occasional grammar Less than 3 All grammar / 10
and organized grammar, spelling error, grammar and / / spelling errors, grammar / spelling are
formal sentence writing style is or spelling generally readable spelling errors, correct and
presentations structure rough and errors. with some rough mature, very well
with accurate immature. spots in writing style. readable style. written.
use of
technical
vocabulary

CLO5/PLO8 Demonstrates Timeliness Report handed Report handed Up to one day late Report handed Report handed 10
punctuality, in in more in time earlier than the
timeliness, more than than two days given time
responsibility three late
and days late.
appropriate

Revised Jan 2019

 communication
etiquette

CLO5/PLO8 Comprehends Precaution No precaution One precaution Two precautions are Three Four or more 10
all the steps steps are is addressed on addressed on the precautions are precautions are
experiment addressed. the following: following: addressed on addressed on
according to 1. Safety 1. Safety the following: the following:
Standard 2. Experiment 2. Experiment SOP 1. Safety 1. Safety
Operating SOP 3. Experimental error 2. Experiment 2. Experiment
Procedures 3. Experimental SOP SOP
(SOP) error 3. Experimental 3. Experimental
error error

Total Mark (100) 100%

Revised Jan 2019

 FACULTY OF ENGINEERING
DEPARTMENT OF CHEMICAL & PETROLEUM ENGINEERING
INDIVIDUAL PRACTICAL ASSESSMENT
Student Name: _________________________________________ Student ID: _____________

Items Unacceptable Satisfactory Moderate Good Excellent

Score
Score 1 2 3 4 5
Problem Unable to identify Give unclear and/or Able to give some Able to give clear Able to give clear
Analysis known and incorrect explanation with explanation with slight and correct
unknown explanation regards some inaccuracy inaccuracy regards to explanation regards
(CLO1/PLO 2) information, to identify known regards to identify identify known and to identify known
uncertainties and and unknown known and unknown information, and unknown
(Interview) biases of the information, unknown uncertainties and information,
experiments. uncertainties and information, biases of the uncertainties and
biases of the uncertainties and experiments. biases of the
experiments. biases of the experiments.
experiments.
Investigation Unable to Able to propose, Able to propose, Able to propose, Able to propose,
propose, justify justify and justify and justify and justify and
(CLO2/PLO 4) and demonstrate demonstrate demonstrate demonstrate demonstrate
appropriate skills appropriate skills appropriate skills appropriate skills appropriate skills
(Observation / and/or strategies and/or strategies and/or strategies and/or strategies and/or strategies
Interview) required by the required by the task required by the task required by the task required by the task
task and makes but makes critical but makes minor without significant without significant
critical errors in errors in applying errors in applying errors. errors and apply
applying them. them. them. them in innovative
ways.
Communication Mumbles the Low voice, often Voice was Clear voice, generally Natural, confident
words, language relies on the note. occasionally effective delivery. delivery that does
(CLO3/PLO 10) was unclear, inaudible; not just convey the
relies exclusively occasionally relies message but
(Interview) on the note. on note. enhances it;
excellent use of
volume.
Individual and No participation. Perform very little Perform some Perform nearly all Perform all duties,
Teamwork duties of assigned duties of assigned duties of assigned leads all discussion
team role or team role & less team role. and group activity.
(CLO4/PLO 9) participated only participated in Participated in nearly
when called on. discussion and all discussion and
(Observation / group activity. group activity.
Interview)
Ethics Up to 20 minutes More than 15 Up to 10 minutes Up to 5 minutes late. Arrive before lab
late. Does not minutes late. late. Conform to Conform to nearly all session. Conform to
(CLO5/PLO 8) conform to lab Conform to nearly nearly all lab lab regulation & all lab regulation &
regulation & all lab regulation & regulation & safety. safety. safety.
(Observation / safety. safety.
Interview)

Total Mark
(out of 25 points)

Total Percentage (20%)

Comments: -
_____________________________________________________________________________________
_____________________________________________________________________________________

[Type text]
Name of Assessor: ____________________ Date & Signature: ____________________