UNIVERSITI KUALA LUMPUR

MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING TECHNOLOGY

LABORATORY REPORT SUBMISSION FORM

To: AZYYATI BINTI JOHARI Subject: CKD 20102 SEPARATION TECHNOLOGY

From: (Student Name) Student ID No. Jotter Note (5 marks)

1. MUHAMMAD DANIEL BIN ISMAIL 1. 55104118010
2. BADRUL AIMAN BIN MOHD 2. 55102118005
3. MUHAMMAD AL-BAIHAQI BIN RAFIDI 3. 55102118010
4. MUHAMMAD AFIQ BIN AZRI 4. 55102118019

Section: LO1-P1 Group No: 4

Title of Experiment: PACKED COLUMN DISTILLATION

Date of Experiment: Date of Submission:

` SUB TOPIC NOTE VERY POOR POOR MODERATE GOOD EXCELLENT

Brief review on the objectives of the experiment, main experimental results and significant discussion
Summary 1 2 5 7 10
and conclusions obtained from the work
Introduction Theoretical of process and description of equipment (limited to 1 page only). 1 2 3 4 5
Objective List of objectives of experiment (rewrite the objectives listed). 1 2 3 4 5
Procedure Simplified procedure (start-up, analysis, experimental). Write in passive sentences. 1 2 5 7 10
Result/Data Tables of results, graph and calculation and sample calculation. 1 5 8 12 15
Discussion Graphical explanation (if any) and further discussion. 5 12 18 24 30
Conclusion Principal outcomes (related with objectives) and recommendation. (2 paragraphs only). 1 2 5 7 10
References At least three (5) references; book, manual, journal and internet sources. Write according to format. 1 2 3 4 5
Raw data during experiment (must be complete, tidy and signed) and any related diagram.
Appendix 1 2 3 4 5
Jotter note (with signature).

TOTAL : 100 marks /100

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1.
Summary/ Abstract
0
*Write in this page only (1 page only).

Basically, this experiment is about operating a Vapour-Liquid Separation

Experiment using a Packed Column Distillation Process Unit. The experiment
began with the preparation of 30 L of sample by mixing 3 L of Ethanol and 27
L of Water together to obtain 30 L of sample. The samples were collected from
the top and bottom from the Sampling Port for every 5 minutes. Besides that
each temperature at temperature transmitter 1 until 6 was recorded in the table
2. The concentration of the samples drawn was measured using the
Refractometer through the Refractive Index method. The reading of
temperatures was recorded for every 5 minutes. After all the data were written
down, the samples can then be analysed in order to determine the Refractive
Index values for both top and bottom products. Initially, the refractive index,
RI of Ethanol had been measured by differing the amount of percentage in
mixture of ethanol and distilled water by 10%, 20%, 30%, 40% and 50% and it
resulted to value of 1.333, 1.337, 1.341, 1.345, and 1.349 respectively
(Table1.0). Proceeded to value of RI at top product ( Ethanol) and value of RI
at bottom product (Water) that had been measured starting from min of 40
(Table 2.0). Regarding to the tabulated result, the values of RI at top product
increased while for values of RI at bottom product became constant. Next, the
concentration of Ethanol also had been calculated and tabulated in Table 3.0. It
then showed that from min of 40 to min of 70, it can be observed that most of
the top product contained 70% of ethanol and it increases as the time increases.
Besides for concentration of Water , it had been calculated and tabulated in
Table 4.0. It can be observed that most of the bottom product contained 7.5%
of ethanol and it remain constant as the time increases. Overally, it can be
observed that as the time increases, the temperature (oC) also increases. It was
also observed from the results that the higher the temperature, the higher the
RI. Higher RI which was close to the standard RI indicates better separation
efficiency. The Refractive Index value was high at the end of the experiment,
showed that the composition of each sample was almost pure ethanol as the RI
was closed to standard RI. However, there were possible errors that can occur

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during the experiment. Firstly, the mixture of ethanol and water was prepared
with concentration of ethanol that less than 10% that leads to inaccurate result.
Besides that there were contaminations in the ethanol sample that contribute to
abnormal results. Next, the cooling water was not supply properly to the
condenser might leads to high temperature of temperature indicator. The
temperature in column might too high that will cause the equipment to have a
leakage. Lastly, the instrument was not at the optimum performances. Thus, the
ideal expected results could not be achieved.

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2.0 Introduction
*Write in this page only (1 page only). Any related diagram, put at Appendices.

Distillation is one of the important unit operations in many chemical

industries and has been used from the inception of chemical and process industry.
Distillation is used for the separation of components in a liquid mixture of volatile
constituents. The Distillation Column is usually a vertical column where the liquid
and vapor phases of the mixture are made to mix and approach equilibrium.
[ CITATION HEN90 \l 1033 ]

The two types of distillations utilized in industry are batch and continuous.
Batch distillation is desirable when small quantities of high valued chemicals need to
be separated. In a batch system, the column can handle different mixtures by simply
changing its operating conditions. In this lab, the packing in the column is rachig rig
glass. The distillation column also contains a condenser, which cools and condenses
the vapor leaving the top of the column. A reboiler is connected to the bottom of the
distillation apparatus and it provides the reboil heat that is necessary for distillation.
[ CITATION CHA09 \l 1033 ]

Figure 2 shows the schematic diagram of the apparatus in this experiment.

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3.0 Objective

 Operate vapour – liquid separation experiment using a Packed Column Distillation unit.
 Analyze the sample of top and bottom product by using Refractometer to obtain the
Refractive Index (RI) in order to determine their respective composition.
 Determine the volume of top product obtained for every experimental time interval.
Determine the composition (mole fraction) of feed, final top and bottom products.

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4. Procedure
0

5. Result/Data
0
*Tabulate/ Redraw the table consists of your result in this space. Attach graph paper (if any) or
sample calculation after this page.

COMPOSITION OF FEED IN MOLE:

WATER=0.9668 M
ETHANOL=0.0332 M
APENDIX 1
REFRACTIVE INDEX MOLE FRACTION OF
(RI) ETHANOL
1.332 0.00
1.334 0.02
1.335 0.03
1.337 0.07
1.339 0.09
1.341 0.11
1.344 0.13
1.346 0.16
1.347 0.17
1.348 0.20
1.348 0.23
1.349 0.27
1.349 0.32
1.350 0.36
1.352 0.42
1.354 0.48
1.356 0.55
1.358 0.64
1.359 0.74
1.361 0.85
1.362 1.00

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1.37
f(x) = 0.03 x + 1.34
1.36 R² = 0.87
1.36

REFRECTIVE INDEX (RI)

1.35
1.35
1.34
1.34
1.33
1.33
1.32
1.32
0.00 0.20 0.40 0.60 0.80 1.00 1.20
MOLE FRACTION OF ETHANOL

FIGURE 1

6. Discussion
0
*Write in 2 pages only.

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The concept of this experiment is distillation. The solution of ethanol and

distilled water will be separated using this process and the composition of the
ethanol will be measured. The result show the reading of refractive index(RI)
of the top product decrease from 1.362 to 1.358 in 35 minutes. The reading for
bottom also decrease from 1.345 to 1.333 and volume of top product which is
pure ethanol also decrease from 465ml to 150ml.
Function of RI reading is to determine how fast light travels through the
material. It can be defined as n=c/v where c is the speed of light in vacuum
and v is the phase velocity of light in the medium. The refractive index also
determines how bent, or refracted, the direction of light is when reaching a
substance. This is defined by Snell's law of refraction, n1 sinning1 = n2
sinning2, where the angles of incidence and refraction of a ray crossing the
interface between two media with refractive indices n1 and n2 are,
respectively, both x1 and x2 (Hecht, Eugene (2002). Optics. Addison-Wesley).
In this experiment RI reading function is to measure the reflux ratio.
Reflux ratio is the ratio between the amount of reflux that goes back down
the distillation column and the amount of reflux that is collected in the
receiver. The importance of reflux ration in distillation process is to explain
the volume we get at the top product. The higher the reflux ratio in the
distillation column, the more vapor/liquid contact may occur. Therefore higher
reflux mean higher distillate purity. Also, it means the distillate production
will be slower.
In this experiment, there are several main component in this plant. One of it
the cooling water that lower the temperature of component in this plant.
Second is the reboiler which is to raise the temperature of ethanol solution.
There are also condenser. Condenser used to condense a gaseous substance
into a liquid state through cooling.
There is several things that can cause the result mess up. First of all is
the solution which is need 3L of pure ethanol and 27L of distilled water. If the
solution was wrong, the result will be broke. Furthermore, the temperature
must be maintained under 100°C by adjust the current of the reboiler to
between 170V-180V. Temperature over 100°C make distillation process
exceed supposed measure.
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7. Conclusion
0

Conclusively, the aims of this experiment which were to operate a Vapour-

Liquid Separation Experiment using a Packed Column Distillation Process
Unit, to prepare a calibration curve for Refractive Index (RI) vs. Mole Fraction
Of Ethanol – Water mixtures, to analyse the sample for the top and bottom
product by Refractometer, to obtain the Refractive Index (RI) in order to
determine their respective composition and to obtain the time when the
Vapour-Liquid Separation is nearly finish. Regarding to the tabulated result,
the values of RI at top product increased until the 15 th minute and then slowly
decreased while for values of RI at bottom product became is not that obvious
change. It can be deduced that the longer the time, the higher the RI for top
product. This was because the ethanol wants to achieve the standard RI of
ethanol which was 1.3614. While for RI values of bottom product, the value
was range about 1.333 to 1.345, thus it showed that it almost achieves the
standard refractive index of water which was 1.3330. It can observe that most
of the bottom product contained 7.5% of ethanol and it remain constant as the
time increases. Hence as the bottom product contained small amount of
ethanol, it can be deduced that the water was successfully separated from the
mixture of ethanol and water. Overally, it can be observed that as the time
increases, the temperature (oC) also increases. It was also observed from the
results that the higher the temperature, the higher the RI. Higher RI which was
close to the standard RI indicates better separation efficiency. The Refractive
Index value was high at the end of the experiment, showed that the
composition of each sample was almost pure ethanol as the RI was closed to
standard RI. As an overall, this experiment was considered as a success.
Based on errors that had been identified, some recommendations have
been proposed in order to reduce them. Firstly, ensure that the percentage of
ethanol and water in the mixture have been calculated correctly so that the
values of RI obtained are synchronized to the increase of percentage of
ethanol. Secondly, ensure that this experiment is conducted in enclosed room
and the apparatus used are clean properly to avoid contamination from

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occurring. Next, the cooling water should be supplied sufficiently so that the
temperature inside the vessel will not become extremely high that could lead
to leakage problem. Lastly, do ensure that the equipment is in optimum
condition so that there is no problems occurred during conducting the
experiment.
8. Reference(s)
0

References
KISTER, H. (1990). Distillation operation.
THOMAS, C. (2009). Introduction to process technology.

Websites

UOLAB.LSU. (2013) Packed Distillation Column

http://www.uolab.lsu.edu/packed_distillation_column.htm

DISTILLATION (2011) Types of Distillation.

http://lorien.ncl.ac.uk/ming/distil/distiltyp.htm

UNKNOWN. (2005) Packed Distillation Column.

http://cuo2.kkft.bme.hu/packed.pdf .

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9. Appendices
0
*Put raw data, signed jotter note and related diagram in this section.

Figure 2: Packed distillation column

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