UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

HEAT & MASS TRANSFER LABORATORY
(CHE504)
NAME: STUDENT NO :
MUHAMAD IBNU HAKIM BIN SHUHAINI 2017632072
MOHAMAD NORAFIQ BIN ZULKEPLI 2017632138
NORHAYATI BINTI AB RAHMAN 2017632114
NURUL NAJIHAH BINTI JAAFAR 2017632056
NURLINA SYAHIIRAH BINTI MD TAHIR 2017632214
GROUP : EH2204I
EXPERIMENT : DISTILLATION COLUMN (L6)(GROUP REPORT)
DATE PERFORMED : 22nd MARCH 2018
SEMESTER :4
PROGRAMME / CODE : CHEMICAL ENGINEERING / EH220
SUBMIT TO : MADAM SYAFIZA BINTI ABD HASHIB

No. Title Allocated Marks (%) Marks

1 Abstract/Summary 5
2 Introduction 5
3 Aims 5
4 Theory 5
5 Apparatus 5
6 Methodology/Procedure 10
7 Results 10
8 Calculations 10
9 Discussion 20
10 Conclusion 10
11 Recommendations 5
12 Reference 5
13 Appendix 5
TOTAL MARKS 100

Remarks:

Checked by: Rechecked by:

--------------------------- ---------------------------

Date: Date:
 TABLE OF CONTENT

1.0 ABSTRACT ................................................................................................................... 2

2.0 INTRODUCTION......................................................................................................... 3

3.0 OBJECTIVES ............................................................................................................... 5

4.0 THEORY ....................................................................................................................... 6

5.0 MATERIALS & APPARATUS ................................................................................... 8

6.0 METHODOLOGY ..................................................................................................... 10

7.0 RESULTS .................................................................................................................... 12

8.0 CALCULATIONS ...................................................................................................... 14

9.0 DISCUSSION .............................................................................................................. 19

10.0 CONCLUSION ........................................................................................................... 21

11.0 RECOMMENDATIONS ............................................................................................ 22

12.0 REFERENCES............................................................................................................ 23

13.0 APPENDICES ............................................................................................................. 24

LAB REPORT ON DISTILLATION COLUMN (L6) 1

1.0 ABSTRACT

Distillation is a separation process where liquid or vapor mixture of two or more substance is
separated into its desired component fractions through boiling and condensation. In this
experiment, mixture of methylcyclohexane (MCH) and toluene were used. This experiment
was conducted to determine pressure drop for various boil-up rates in a batch distillation, the
degree of foaming on trays each time the power increased and the measurement of Refractive
Index. There are two parts of experiments were conducted which were determining pressure
drop in batch distillation and determining unknown concentration. With the aim of getting
pressure drop of the column, the power was set up to 0.5kW, 0.75kW, 1.00kW, and 1.25kW.
For every power, 100mL of sample was collected to measure the Refractive Index. It is
observed the degree of foaming was increased with the increment of power. For experiment
B, pure MCH, pure toluene, 25% MCH, 50% MCH and 75% MCH were tested for their
Refractive Index to compare the value with the previous sample from experiment A. It can be
concluded that this experiment has achieved its objectives which is the boil-up rates depend
on the heater power used. The greater the heater power, the higher the boil-up rates will be
and the refractive index values shows an increment when the power input increase.

LAB REPORT ON DISTILLATION COLUMN (L6) 2

2.0 INTRODUCTION

Separation process consist of distillation that can purified the organic liquid. This process
separating mixture into two or more products that consist of different boiling points through
the vaporization of a liquid mixture components and the recycling of counter-current gas
liquid flow in the column. Therefore, the liquid phase richer is less volatile which has higher
boiling point and the vapor phase is more volatile with the lower boiling point component.
Distillation process is the most of common separation used in industry because its known as
90% efficiency in separation process and significantly user of energy in the heating process
that necessarily involved. The apparatus used in the distillation process is Distillation
Column.

The column of the distillation column has many types of tray such as bubble cap
trays, sieve tray and packed bed column. The principal of bubble cap tray is not a counter
current flow but cross flow on every stage while sieve tray flow with counter current flow.
Furthermore, packing column can have a lower pressure drop and good for thermally
sensitive liquid. To determine the appropriate tray, it will consider the fouling tendency,
allowable of pressure drop and turndown requirement in the column.

(a) (b)
Figure 1 - (a) Packing Columns (b) Bubble Cap Tray, Sieve Tray, Valve Tray

The separation of distillation process that use heating power can separate the vapor
and liquid phase. Heating element installed at the bottom of to ensure the liquid mixture
evaporates in the whole column. The vapor phase will rise up into the condenser and the
product will be entering into the distillate tank, meanwhile the liquid will go downward as a
waste or bottom products. There are two heat exchangers above the distillation column. The
function of the second exchanger acts as condenser which allow the vapor leaving the first

LAB REPORT ON DISTILLATION COLUMN (L6) 3

exchanger using cooling water. Then the reflux tank will be filled with the condensate that
flow from condenser. The electromagnetic controlled in the column by switching of on and
off controlled the reflux ratio. The remaining from the reflux tank then turned back to the top
of the column. The separation behaviour of the column can be analysed by the sample’s
analysed for each stage. Therefore, the refractive index of every sample analysed by refractor
meter. The rectification is the mass transfer between the two phases in equilibrium.

Figure 2 - Process Flow Diagram for Common Distillation Column Process

From the distillation column system, there are two principle method that need to be
followed in order to carry out the experiment which is batch distillation method and
continuous steady state distillation process. Batch distillation process is the process when
there is no reflux and the vapor that boiling the liquid mixture to be separated and condensing
vapor not allowing any liquid to return into the top column. Therefore, the continuous
distillation process is vice versa. Some example of continuous distillation is flash distillation
(single stage partial vaporization) and rectification distillation.

In the industries, there are many categories of products that use distillation for
separation such as petroleum refining, petrochemical, process of natural gas and beverage. In
generally, the typical aim to remove the light component from mixture of heavy component.
Other example of distillation process is within the food industries which concentrating
essential oils and flavour, deodorization of fats and oil.

LAB REPORT ON DISTILLATION COLUMN (L6) 4

3.0 OBJECTIVES

The two (2) main objectives for this experiment are:

1) To determine the pressure drop over the distillation column for various boil-up rate.
2) To determine the mixture compositions by using refractometer.

LAB REPORT ON DISTILLATION COLUMN (L6) 5

4.0 THEORY

The unit operation distillation is a method used to separate the components of a liquid
solution, which depends upon the distribution of these various components between a vapor
and liquid phase (Geankoplis,1993). Distillation is a physical process used to separate
chemicals from a mixture depending on the differences in volatilities of the components that
make up the mixture. In the distillation process, a volatile vapor phase and a liquid phase that
vaporizes are involved (Geankoplis, 1993). Their operation is based on the difference in
boiling temperatures of the liquid mixture components.

The boiling point of methylcyclohexane is 101°C (PubChem, 1997) while toluene is

111°C (PubChem, 2002). The binary mixture of methylcyclohexane-toluene is used in the
experiment to understand the concept of distillation.

VMCH (ρMCH )
MWMCH
Composition of Methylcyclohexane, XMCH =
VMCH (ρMCH ) VolumeTol (ρTol )
+
MWMCH MWTol

Where,
VMCH = Volume of Methylcyclohexane, mL
VTol = Volume of Toluene, mL
MWMCH = Molecular Weight of Methylcyclohexane, 98.189g/mol (PubChem, 1997)
MWTol = Molecular Weight of Toluene, 92.141g/mol (PubChem, 2002)
ρMCH = Density of Methylcyclohexane, 770 kg/m3
ρTol = Density of Toluene, 867 kg/m3

The methycyclohexane-toluene mixture is heated at varying boil-up rate which is

done by varying the power input to the reboiler.

mL Volume of Condensate (mL)

Boil − up Rate ( )=
min Time Taken To Collect Condensate (min)

The most volatile component will vaporized first for which in this case is the
methylcyclohexane until they reach equilibrium. The vapor raised in the boiler flow into the
unit at the bottom of the column. The velocity of the vapor passing through the column
depends on the boil-up rate. As the vapor passes straight upward through the liquid on the
sieve trays (Tham M. T., 1997), resctriction occurs on the holes of the trays causing pressure
drop.

LAB REPORT ON DISTILLATION COLUMN (L6) 6

 The total pressure drop across each tray is the sum of that caused by the restriction of
the holes in the sieve tray and that caused by passing through the liquid (foam) on top of the
tray. The pressure drop is expected to increase as the boil – up rate is increases. As the vapor
exits the top of the unit, it is cooled by a condenser (Tham M. T., 1997). The condensate is
stored in the reflux drum.

The refractive indexes can be measured for mixtures of known concentration made up
for the binary system. The refractometer works using the principle of light refraction through
liquids (ProSciTech, 2014). It measure the critical angle of the liquid or mixture under test
and different concentration will yield to different reading of the critical angle. Critical angle
is the maximum angle of incident for refraction to still occur which angle of refraction of 90°
from denser to less dense medium (Prisms, n.d.).

LAB REPORT ON DISTILLATION COLUMN (L6) 7

5.0 MATERIALS & APPARATUS

5.1 Materials
1) 10L 50 mole percent Methylcyclohexane – 50 mole percent Toluene
2) Pure methylcyclohexane
3) Pure Toluene
4) 25 mole percent, 50 mole percent and 75 mole percent methylcyclohexane
5) Distilled water

5.2 Apparatus
1) Continuous Distillation Column (UOP3CC)
2) 100mL measuring cylinder
3) Stopwatch
4) Automatic Digital Refractometer RX-5000𝛼
5) Dropper
6) 250mL Beaker

Cover Plate
Sample Stage

Rugged Metal Body

Measurement Principle
Touch screen

Figure 3 - Digital Refractometer using the principle that as density increases, the
refractive index rises proportinately (Automatic Digital Refractometer RX-5000a, n.d.)

LAB REPORT ON DISTILLATION COLUMN (L6) 8

 T12
CONDENSER VENT

T11

DECANTER

V8
REFLUX
VALVE F11
V10
T
T10
V7 V5
COLUMN V14
T1
T13
T2 TOP
T3 V3 PRODUCT COOLING
MANOMETER T4 RECEIVER WATER
P1
E-4
T5 V12 V4 V15
T6 FEED TANKS
T7
T8 VACUUM
PUMP
V6
T14

T9 T
REBOILER FEED PUMP
T
V1
HEATER
V2
HEAT
EXCHANGER
BOTTOM
PRODUCT
RECEIVER

Figure 4- P&ID for UOP3CC Continuous Distillation Column Used in the Experiment

LAB REPORT ON DISTILLATION COLUMN (L6) 9

6.0 METHODOLOGY

6.1 General Start Up

1) The electrical power to control console was switched on by moving the ELCB
switch to the UP position. The lamp in the reboiler which is LOW LEVEL lamp
section of console illuminated along with the reboiler power, reflux timer, column
temperature and process temperature displays.
2) All the valves (V1 to V15) were in closed position
3) The laboratory cold water supply turned on and the control flow valve(V5)
opened to give maximum flow into the condenser via flowmeter(F11). The leaks
were checked.
4) The manometer tub filled until an equal level is visible approximately halfway up
the scale. The V6 and V7 closed.
5) The reboiler heater power was switched on at the console and the power adjusted
to the heater 1.50Kw. The water in the reboiler begin to heat up and observed by
the selecting (T9) on the process temperature digital display.
6) Valve V6 and V7 were opened and the pressure difference in the manometer
observed. Then V6 and V7 closed.

6.2 Experiment A
1) The experiment started when the power of control panel was turned on and all the
valves were closed except valve 10 on the reflux pipe and the boiler filled with 10
litres of mixture to be distilled.
2) The temperature selector switch was set to T9 which is the temperature in the
reboiler.
3) Valve V5 was opened and admitted the cooling water to the condenser
approximately 3 litre/min.
4) When the control panel has been turned on the power controller, the reboiler
heating element that fully anticlockwise was switched by the turning on power
heating element to ‘power’ on position.
5) The reading of power approximately 0.5kW was set on the power controller and
then the content of the reboiler was warmed up which observed on the
temperature readout meter for 10 minutes heating.

LAB REPORT ON DISTILLATION COLUMN (L6) 10

 6) After 10 minutes valve V6 and V7 were opened so that the pressure drops
obtained on the manometer for top and bottom. The overall pressure drop was
recorded.
7) On the top of the column, the cool distillate was returned and cascade down the
trays and formed a liquid level on the trays while the bubbling vapour passed
through the liquid on that trays. The degree of forming was observed and
recorded.
8) The sample of 100ml was collected through valve V3 (opened valve) using
measuring cylinder, meanwhile the collecting time of the sample was recorded
and the boil-up rate (L/hr) was calculated based on the time taken.
9) The refractive index (RI) of the collected sample was obtained by test using
Refractometer. The refractometer was being calibrated by zeroing the instrument
using distilled water before RI testing.
10) The higher power of 0.75KW, 0.10KW and 1.25KW used for the repeated
experiment.

6.3 General Shut Down

1) The heater power, feed pump motor and reflux valve at the console was switched
off.
2) The equipment was disconnected from electrical supply when the equipment not
used.
3) All the water from the system was drained using the drain valves V2, V3, V4,
V11 and by breaking the pipe connections of the bottoms product cooler and feed
pump.

6.4 Experiment B
1) The volume of constituent was calculated.
2) R.I. measured with the makeup of small quantities of 25 mole percent, 50mol
percent, 75 mole percent and 100 mole percent methyl cyclohexane.
3) The refractive index (R.I) of pure methyl cyclohexane and pure toluene was
measured.

LAB REPORT ON DISTILLATION COLUMN (L6) 11

7.0 RESULTS

Table 7.1: Experiment A (Determining Column Pressure Drop)

Power Boil-Up Rate Pressure Drop Degree Of Foaming RI
(kW) (L/hr) (cm H20)
0.50 2.7273 62 Gently localized 1.4376
0.75 7.6596 61 Foaming Violently over the tray 1.4377
1.00 51.4286 217 Foaming Violently over the tray 1.4519
1.25 90.0000 211 Foaming Violently over the tray 1.4582
1.50 - - - -
1.75 - - - -

PRESSURE DROP VS BOIL-UP RATE

250

200
Pressure Drop (cm H2O)

150

100

50

0
0 10 20 30 40 50 60 70 80 90 100
Boil-up Rate (L/hr)

Figure 5 - Graph of Pressure Drop vs Boil Up Rate

The graph undergoes slight drop at the beginning and then increases sharply before it
goes for slight drop again.

LAB REPORT ON DISTILLATION COLUMN (L6) 12

Table 7.2: Experiment B (Determining Mixture Composition)
Concentration of Volume Refractive
Methylcyclohexane (mL) Index
(%) Toluene Methylcyclohexane
0% 100.0000 0.0000 1.4964
25% 71.5375 28.4625 1.4746
50% 45.5871 54.4129 1.4549
75% 21.8261 78.1739 1.4577
100% 0.0000 100.0000 1.4234

REFRACTIVE INDEX VS MOLE FRACTION OF

MCH
1.5100
1.5000
REFRACTIVE INDEX

1.4900
1.4800
1.4700
1.4600
1.4500
1.4400
1.4300
1.4200
1.4100
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 1.00 1.10
MOLE FRACTION OF MCH

Figure 6 - Graph of Refractive Index vs Mole Fraction of MCH

The graph shows a steady drop until 0.50 mole fraction of methylcyclohexane and
slight increases up to 0.7 mole fraction of methylcyclohexane before it drop steadily again
until it reach the pure concentration of methylcyclohexane.

LAB REPORT ON DISTILLATION COLUMN (L6) 13

8.0 CALCULATIONS

Experiment A: Determining Column Pressure Drop

Table 8.1: Pressure drop

Pressure Drop (cm H2O)

Power (kW)
Top Bottom Pressure Difference
0.50 163 101 62
0.75 163 102 61
1.00 240 23 217
1.25 237 26 211

Table 8.2: Refractive index

Refractive Index
Power (kW)
Reading 1 Reading 2 Average
0.50 1.43754 1.43755 1.43755
0.75 1.43791 1.43747 1.43769
1.00 1.45185 1.45184 1.45185
1.25 1.45809 1.45833 1.45821

1) Boiler-up rate (L/hr)

𝐕𝐨𝐥𝐮𝐦𝐞(𝐋)
𝐁𝐨𝐢𝐥 − 𝐮𝐩 𝐫𝐚𝐭𝐞 =
𝐓𝐢𝐦𝐞(𝐡𝐫)
Volume:
100 mL = 0.1 L

i. 0.50 kW
0.1 L
Boil − up rate =
1 hr
2.2 min ×
60 min
L
= 2.7273
hr

LAB REPORT ON DISTILLATION COLUMN (L6) 14

 ii. 0.75 kW
0.1 L
Boil − up rate =
1 hr
47 s ×
3600 s
L
= 7.6596
hr

iii. 1.00 kW
0.1 L
Boil − up rate =
1 hr
7s×
3600 s
L
= 51.4286
hr

iv. 1.25 kW
0.1 L
Boil − up rate =
1 hr
4s×
3600 s
L
= 90
hr

Experiment B: Determining the mixture compositions

Molecular weight of Methylcyclohexane = 98.19 g/mol

Molecular weight of Toluene = 92.15 g/mol

Density of Methylcyclohexane = 0.774 g/m3

Density of Toluene = 0.867 g/m3

VolMCH × ρMCH × 100

MWMCH
Concentration =
VolMCH × ρMCH Voltol × ρtol
+
MWMCH MWtol

100
=
Voltol MWMCH ρ
1+ × × tol
VolMCH MWtol ρMCH

LAB REPORT ON DISTILLATION COLUMN (L6) 15

For 100 mL of mixture solution, the quantity required:

i. 100% Methylcyclohexane : 0% Toluene

VolMCH + Voltol = 100 mL
When the mixture solution has 100% Methylcyclohexane, we can neglect the volume
of toluene. Therefore,
VolMCH + 0 = 100 mL
VolMCH = 100 mL
Voltol = 0 mL

ii. 75% Methylcyclohexane : 25% Toluene

100
75 =
Voltol 98.19 0.867
1+ × ×
VolMCH 92.15 0.774
Voltol
1.3333 = 1 + × 1.1936
VolMCH
Voltol
0.3333 = × 1.1936
VolMCH
Voltol
0.2792 =
VolMCH
1 Voltol = 0.2792 VolMCH

Therefore,
VolMCH + Voltol = 100 mL
1 VolMCH + 0.2792 VolMCH = 100 mL
1.2792 VolMCH = 100 mL
VolMCH = 78.1739 mL
Voltol = 21.8261 mL

LAB REPORT ON DISTILLATION COLUMN (L6) 16

iii. 50% Methylcyclohexane : 50% Toluene
100
50 =
Voltol 98.19 0.867
1+ × ×
VolMCH 92.15 0.774
Voltol
2=1+ × 1.1936
VolMCH
Voltol
1= × 1.1936
VolMCH
Voltol
0.8378 =
VolMCH
1 Voltol = 0.8378 VolMCH
Therefore,
VolMCH + Voltol = 100 mL
1 VolMCH + 0.8378 VolMCH = 100 mL
1.8378 VolMCH = 100 mL
VolMCH = 54.4129 mL
Voltol = 45.5871 mL

iv. 25% Methycyclohexane : 75% Toluene

100
25 =
Voltol 98.19 0.867
1+ × ×
VolMCH 92.15 0.774
Voltol
4=1+ × 1.1936
VolMCH
Voltol
3= × 1.1936
VolMCH
Voltol
2.5134 =
VolMCH
1 Voltol = 2.5134 VolMCH

Therefore,
VolMCH + Voltol = 100 mL
1 VolMCH + 2.5134 VolMCH = 100 mL
3.5134 VolMCH = 100 mL
VolMCH = 28.4625 mL
Voltol = 71.5375 mL

LAB REPORT ON DISTILLATION COLUMN (L6) 17

 v. 0% Methylcyclohexane : 100% Toluene
VolMCH + Voltol = 100 mL
When the mixture solution has 100% Toluene, we can neglect the volume of
Methylcyclohexane. Therefore,
0 + Voltol = 100 mL
Voltol = 100 mL
VolMCH = 0 mL

Table 8.3: Average Refractive Index Of Methylcyclohexane

Refractive Index
Concentration
Reading 1 Reading 2 Average
100% 1.42341 1.42343 1.42342
75% 1.43768 1.43773 1.45771
50% 1.45488 1.45498 1.45493
25% 1.47446 1.47477 1.47462
0% 1.49634 1.49642 1.49638

LAB REPORT ON DISTILLATION COLUMN (L6) 18

9.0 DISCUSSION

Fraction or stage distillation with reflux, from a simplified form of view is considered to be a
process which series of flash-vaporization are arranged in such manner that the vapor and
liquid product counter current to each other at each of the stages. The degree of separation of
the liquid mixture depends greatly on the volatility of one component to the others. The most
volatile component will be boiled as vapor thus separating it with the least volatile
component. The liquid product will be collected at the bottom and the vapor product will be
collected at the top part of the distillation column.

This experiment was divided into 2 parts, experiment A and experiment B

respectively. The main objective of experiment A is to determine the pressure drop over the
distillation column for various boil-up rates. A mixture of toluene and Methylcyclohexane
were fed into the distillation column and were boiled up by using different power input. From
the result obtained from conducting experiment A, graph of pressure drop versus boil up rare
as in Figure 5 is plotted. From that, we can see that the graph undergoes slight drop at the
beginning and then increases sharply before it goes for slight drop again. The drop pattern of
the graph is probably caused by error in which the value of the pressure drop were taken.
Supposedly, the value shown on the manometer were let to stabilize first before the value
could be taken to ensure accuracy of data.

Besides that, the varying power input will also affect the degree of foaming, and the
refractive index of the system. The degree of foaming varies as the power input were set
differently. At 0.5 kW, the foaming at the trays were observed to be at “gently localised”
state but at 0.75 kW, 1.00 kW, and 1.25 kW, the degree of foaming were observed to be at
“foaming violently over the trays” state. The different degree of foaming is dependent on the
upward vapor flow. The higher the power input, the higher the upward vapor flow thus
resulting more ‘violent’ degree of foaming. Apart from that, the refractive index of the
mixture was observed to increases when the power input increases. The refractive index value
of the condensate from Experiment A is taken to compare with the calibration curve from
Experiment B.

As for experiment B, the main objective is to determine the refractive index of MCH
for the calibration curve. Samples with different MCH mole fraction were prepared and each
of the samples refractive index were measured by using refractometer. From the result
obtained from conducting experiment B, graph of refractive index versus mole fraction of

LAB REPORT ON DISTILLATION COLUMN (L6) 19

methylcyclohexane as in Figure 6 is plotted. Based on the graph, we can see that the graph
undergoes steady drop and sudden increases before it drop steadily again. The sudden
increases is probably caused by error in which the reading were taken from the refractometer.
Supposedly, the sample stage were clean properly before the next reading can be taken. This
to ensure that the current sample was not mixed with the previous sample as it can affect the
refractive property of the sample.

Comparing with the calibration curve from Experiment B, the refractive index of the
condensates from Experiment A, shows that the major constituent of the top product of the
distillation column is methylcyclohexane since the refractive index value is closer to that of
high concentration of methylcyclohexane. However based on the results, as the power input
is increases, the composition of the major constituent is also changing. At higher boil – up
rate, the rate vaporization of toluene increases overcoming the rate of vaporization of
methylcyclohexane resulting in refractive index showing the pattern to go closer towards that
of pure toluene.

Since the feed is only fed once where we continue using the balance for the first
power input for the next one, as methylcyclohexane is mostly vaporizes since the boiling
point is lower than toluene, this could also lead to the fact that the value of the refractive
index of the condensates at Experiment A are much closer to that of pure toluene as the
power input is increases. Thus, making as the experiment goes on, the balance of the binary
mixture feed in the reboiler contained mainly of toluene.

LAB REPORT ON DISTILLATION COLUMN (L6) 20

10.0 CONCLUSION

As conclusion, this experiment has achieved their objective which was to determine the
pressure drop over the distillation column for various boil-up rates and to determine the
mixture compositions by using refractometer which set up to two parts. From the experiment
A, the boil-up rates depend on the heater power used. The greater the heater power, the
higher the boil-up rates will be. The boil-up rates are measured by getting the time taken for
the volume of distillate to reach 100 mL, as the temperature increase, the time taken to
reached 100 mL is decreasing. As the refractive index values are also recorded and there are
increasing when the power input increase. For the experiment B, graph 7.2 shows the
relationship between the mixture composition or mole fraction of methylcyclohexane with
their refractive index. From the graph, it shows that the graph undergoes steady drop and
sudden increases before it drop steadily again.

LAB REPORT ON DISTILLATION COLUMN (L6) 21

11.0 RECOMMENDATIONS

There are several recommendations that should be followed while conducting this experiment
in order to get more accurate data. Firstly, each time after collecting the sample, immediately
close the vial to prevent unnecessary evaporation of methylcyclohexane. Secondly, it is
recommended to use glove while collecting the sample as the sample is still hot. Thirdly,
each time to measure the refractive index of the samples, clean the surface of refractometer
using distilled water. Lastly, for the following experiment after measuring the refractive
index of the sample, make sure to put the mixture back into the inlet for reuse.

LAB REPORT ON DISTILLATION COLUMN (L6) 22

12.0 REFERENCES

Automatic Digital Refractometer RX-5000a. (n.d.). (ATAGO) Retrieved 31 March, 2018,

from ATAGO: http://www.atago.net/product/?l=en&k=ABd54879&p=1
Brian Vandagriff, M. M. (30 November, 1998). Engineering 435 Lab Report : Distillation
Column. Retrieved 29 March, 2018, from Laboratories Without Borders:
http://chem.engr.utc.edu/engr435/Distill/distreport-98.htm
Database, P. C. (Ed.). (July, 1997). Methylcyclohexane. (N. C. Information, Producer)
Retrieved 28 March, 2018, from https://pubchem.ncbi.nlm.nih.gov/compound/7962
Database, P. C. (Ed.). (October, 2002). Toluene. (N. C. Information, Producer) Retrieved 28
March, 2018, from https://pubchem.ncbi.nlm.nih.gov/compound/1140
Distillation Project. (15 July, 2017). Retrieved 29 March, 2018, from NTNU Det Skapende
Universitet:
http://folk.ntnu.no/skoge/diplom/prosjekt09/mar/Distillation%20project.pdf
Geankoplis, C. J. (1993). Simple Distillation Methods. In Transport Procesess and Unit
Operations (3rd Edition ed., p. 644). Minnesota: Prentice Hall.
Geankoplis, C. J. (1993). Types of Separation Processes and Methods. In Transport
Processes and Unit Operations (3rd Edition ed., p. 585). Minnesota: Prentice Hall.
Ltd, P. P. (11 October, 2014). Refractometer. Retrieved 28 March, 2018, from Laboratory
Resource: https://laboratoryresource.com/?navaction=getitem&id=174
Prisms. (n.d.). The Critical Angle. Retrieved 28 March, 2018, from The Physics Classroom:
http://www.physicsclassroom.com/class/refrn/Lesson-3/The-Critical-Angle
Tham, M. T. (October, 1997). Basic Distillatrion Equipment and Operation. Retrieved 28
March, 2018, from COSTELLO: http://www.rccostello.com/distil/distileqp.htm
Tham, M. T. (October, 1997). Column Internals. (I. R. C. Costello & Associates, Producer)
Retrieved 28 March, 2018, from COSTELLO:
http://www.rccostello.com/distil/distilint.htm

LAB REPORT ON DISTILLATION COLUMN (L6) 23

13.0 APPENDICES

Figure 7 - Distillation Column Unit Operation Used in The Experiment

(Batch Distillation)

Figure 8 - Digital Refractometer RX-5000a Used in The Experiment

LAB REPORT ON DISTILLATION COLUMN (L6) 24

 Figure 9 – Methylcyclohexane and Toluene Used in The Experiment

LAB REPORT ON DISTILLATION COLUMN (L6) 25

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