Unit Op Lab Example PDF

UNIT OPERATION LAB
(BKF3731)
2017/2018 Semester II
Title of Experiment : Crystallization
Date of Experiment : 10 April 2018
Instructor’s Name : Dr. Sumaiya Bt Zainal Abidin @ Murad
List of Students :
Name Student’s ID
1. Arics Chieng Kie Siong KA15073
2. Rhakesh a/l Gandhi KA15133
3. Lim Hui Lun KA15184
4. Divya Nandhini KA17343
Group No. :3
Section : 02
Marks :
FACULTY OF CHEMICAL AND NATURAL RESOURCES ENGINEERING
UNIVERSITI MALAYSIA PAHANG
Please keep for student reference.
Submitted by; Received by;
(ARICS CHIENG KIE SIONG) ( )
Subject Code : BKF3731 Date Submitted: 17 April 2018
Title of Experiment : Crystallization

TABLE OF CONTENT
No. Title Page
1.0 Abstract 1
2.0 Introduction 2
3.0 Methodology 4
4.0 Results and Discussions 6
5.0 Conclusion and Recommendation 13
6.0 References 14
7.0 Appendices 15
1.0 ABSTRACT
Crystallization was a process where solid particles were formed from a homogeneous
solution. The objective of this experiment was to determine the dissolution enthalpy and
entropy of Epsom salt in acetone, ethanol and water through Van’t Hoff Equation. It also aimed
to study the crystal shape of sugar, copper sulphate and Epsom salt in water. Moreover, this
experiment was conducted to study the recrystallization of Epsom salt by using ice batch and
natural cooling crystallization. The first experiment was started by preparing 10 mL of acetone
and poured into a beaker on a hot plate. Epsom salt was added slowly and stirred well until in
excess at 30 oC, 40 oC and 50 oC. Acetone with saturated Epsom salt in beaker was filtered and
the remaining solution was collected in the crucible. This experiment was repeated with ethanol
and water solvent. Nine crucibles were placed in the furnace for drying overnight. Mass of
Epsom salt after recrystallization were weighed and recorded and the shapes of crystal formed
were observed. Next, the second experiment was began in which sugar was poured into 10 mL
of distilled water at 50 oC until it became saturated solution. This experiment was repeated with
copper sulphate and Epsom salt. Three beakers with filtered saturated solution were poured
into a crucible each. It was then placed in the furnace for drying overnight. The weight of the
crystals after recrystallization were weighed and recorded and the shapes of crystal formed
were observed. The third experiment was carried out by preparing two set of beakers filled
with 50 mL of distilled water and the Epsom salt was added into each beaker until it became a
saturated solution. The first beaker was put under room temperature for natural cooling whereas
the second beaker was kept in an ice batch for crash cooling. In one-minute time interval, the
temperature of each solution in the beaker were recorded. The formation of crystals in each
beaker were also observed. Based on the result, the higher the temperature, the higher the
solubility due to higher kinetic energy gained by the solvent molecules to break apart the
intermolecular attractions between solutes. Next, water solvent had the highest solubility of
Epsom salt (1.204 g/mL), followed by ethanol (1.018 g/mL) and acetone (0.900 g/mL) at high
temperature of 50oC because Epsom salt had higher solubility in water as both of water and
salt were more compatible to form ionic compounds. Moreover, Epsom salt was less soluble
in acetone because it was significantly less polar than water and ethanol. Besides, the Van’t
Hoff plot showed a negative slope which indicated that this experiment was an endothermic
reaction for all different type of solvents. Acetone had the highest dissolution enthalpy of
Epsom salt (21346.195 J/mol) which implied that the reaction absorbed massive heat for the
reaction, followed by ethanol (17850.158 J/mol) and water (10471.483 J/mol). The dissolution
entropy of Epsom salt was found to be 35.3927 J/mol.K, 46.5526 J/mol.K and 16.7885 J/mol.K
for acetone, ethanol and water respectively. Furthermore, the crystal shape of sugar, copper
sulphate and Epsom salt in distilled water were found to appear in monoclinic, triclinic and
orthorhombic lattice structure respectively. In addition, it was noticed that large amount of
crystal was formed at 15th onwards during ice bath cooling as the cold condition promoted the
crystal growth whereas there was no crystal forming during natural cooling. To improve the
accuracy of solubility reading, the Epsom salt in the solvent must be stirred at higher speed to
minimize the mass transfer resistance between the salt and solvent.
2.0 INTRODUCTION
Crystallization was the physical transformation (phase transition) of a liquid, solution,
or gas to a crystal, which was a solid with an ordered internal arrangement of molecules, ions,
or atoms. In other word, crystallization was a technique which chemists used to purify solid
compounds. It was one of the fundamental procedures each chemist must master to become
proficient in the laboratory. Crystallization was based on the principles of solubility:
compounds (solutes) tend to be more soluble in hot liquids (solvents) than they were in cold
liquids. If a saturated hot solution was allowed to cool, the solute was no longer soluble in the
solvent and formed crystals of pure compound. Impurities were excluded from the growing
crystals and the pure solid crystals can be separated from the dissolved impurities by filtration
(L. Yu & S.M. Reutzel-Edens, 2003).
The general process for the crystallization of a solid can be broken down into seven
distinct steps which were solvent selection, dissolution, decolorization, filtration (impurities),
crystallization, filtration (compound) and last one was drying. To crystallize an impure, solid
compound, just added enough hot solvent to it to completely dissolve it. The flask then
contained a hot solution, in which solute molecules - both the desired compound and impurities
- moved freely among the hot solvent molecules. As the solution cooled, the solvent can no
longer held all the solute molecules, and they began to leave the solution and formed solid
crystals. During this cooling, each solute molecule in turn approached a growing crystal and
rested on the crystal surface. If the geometry of the molecule fitted that of the crystal, it will be
more likely to remain on the crystal than it was to go back into the solution. Therefore, each
growing crystal consisted of only one type of molecule, the solute. After the solution had came
to room temperature, it was carefully set in an ice bath to complete the crystallization process.
The chilled solution was then filtered to isolate the pure crystals and the crystals were rinsed
with chilled solvent (Zurich, 2008).
In cooling crystallization, the supersaturation was created by a decrease in temperature.
Depending on how the solution was cooled, a different product was obtained. The simplest way
of performing a cooling crystallization was to let a warm solution cooled to the surrounding
room temperature. Obviously, the cooling rate will be highest in the beginning, when there was
a large temperature difference between the solution and its surroundings, and it will be lowest
at the end of the crystallization (Zurich, 2008).
The general advantages of crystallization as a process were high purification can be

obtained in a single step. Besides, it may be more economic than alternative separation
processes. Crystallization was used industrially in a wide variety of processes. Typical
applications included bulk chemicals, such as salt, sugar and fertilizers; high value-added
products such as specialty chemicals and pharmaceuticals; and difficult separations such as
ortho- and para-xylene (Hallas N.J., 2011).
3.0 METHODOLOGY
Materials : Epsom Salt, Sugar, Copper Sulphate, Ethanol, Acetone, Water
Apparatus : 50 mL beaker, 1 L beaker, Weighing Balance, Filter Paper, Filter Tunnel,
Hot Plate, Spatula, Magnetic Stirrer and Crucibles
3.1 Epsom Salt in Acetone, Ethanol and Water Solvent Under Furnace
Nine empty crucibles were cleaned, weighed and labelled as different solvents for 3 different
temperatures of 30 oC, 40 oC and 50 oC.
30 mL of pure acetone, ethanol and water solvents were prepared and labelled in beakers respectively.
10 mL of acetone was measured using measuring cylinder and poured into a beaker on a hot plate.
Epsom salt was added slowly and stirred well until in excess at the temperatures of 30 oC, 40 oC and
50 oC. Acetone with saturated Epsom salt in beaker was filtered to remove the excess salt and the
remaining solution was collected in the crucible. The weight of the crucible before drying was
weighed and recorded.
Step 3 and 4 were repeated with ethanol and water solvent.
Nine crucibles were placed in the furnace for drying overnight. The crucibles were wrapped with
aluminium foil.
Mass of Epsom salt after recrystallization under different conditions were weighed and recorded.
After salt crystal formation, the shapes of crystal formed were observed and photos were taken for
record.
3.2 Sugar, Copper Sulphate and Epsom Salt in Distilled Water Under Furnace
Three empty crucibles were cleaned, weighed and labelled for sugar, copper sulphate and Epsom salt
solvents.
Sugar was poured into 10 mL of distilled water at 50 oC until it became saturated solution. The
solution was stirred well until all the solute was well dissolved and in excess.
The saturated solution was filtered to remove the excess salt.
Step 1 and 2 were repeated with copper sulphate and Epsom salt.
Three beakers with filtered saturated solution were poured into a crucible each and the weight of
crucibles before drying were weighed and recorded.
Three crucibles were placed in the furnace for drying purpose overnight. The crucibles were covered
with aluminium foil.
The weight of the crystals after recrystallization were weighed and recorded.
After salt crystal formation, the shapes of crystal formed observed and photos were taken for record.
3.3 Crash Cooling vs Natural Cooling Crystallization
Two set of beakers were filled with 50 mL of distilled water and the Epsom salt was added into each
beaker until it became a saturated solution. Both solutions were stirred thoroughly to ensure it was
homogeneously mixed.
The first beaker was put under room temperature for natural cooling. The second beaker was kept in
an ice batch for crash cooling.
In one-minute time interval, the temperature of each solution in the beaker were recorded. The
formation of crystals in each beaker were also observed.
4.0 RESULTS AND DISCUSSIONS
4.1 Dissolution Enthalpy and Entropy of Epsom Salt
Volume: 10 mL
Table 4.1: Experimental Results of Epsom Salt at Different Temperature in Acetone, Ethanol
and Water
Solvent Temperature Empty Wet Dry Solubility Dissolution Dissolution
Crucible Weight Weight (g/mL) Enthalpy, Entropy,
Weight (g) (g) ∆𝑯 ∆𝑺
(g) (J/mol) (J/mol.K)
Acetone T1 = 30 oC 35.4689 36.0310 35.7889 0.032 21346.195 35.3927

T2 = 40 oC 31.4490 32.3982 31.8290 0.038
T3 = 50 oC 29.9836 31.2925 30.5236 0.054
Ethanol T1 = 30 oC 29.9529 36.1635 33.6329 0.368 17850.158 46.5526
T2 = 40 oC 29.7811 37.5595 35.3111 0.553
o
T3 = 50 C 35.3935 44.7956 42.0535 0.666
Water T1 = 30 oC 36.6308 50.0707 45.6308 0.900 10471.483 16.7885
T2 = 40 oC 28.9188 44.4527 39.0988 1.018
o
T3 = 50 C 35.3715 52.8364 47.4115 1.204
Based on the result, the solubility of the salt was calculated using equation below:
𝐷𝑟𝑦 𝑊𝑒𝑖𝑔ℎ𝑡 (𝑔)−𝐸𝑚𝑝𝑡𝑦 𝐶𝑟𝑢𝑐𝑖𝑏𝑙𝑒 𝑊𝑒𝑖𝑔ℎ𝑡 (𝑔)
Solubility =
10 𝑚𝐿
Solubility of Epsom Salt in Different Type of Solvents versus

Temperature
1.4
1.2
Solubility (g/mL)
0.8
0.6
0.4
0.2
0
0 10 20 30 40 50 60
Temperature (oC)
Acetone Ethanol Water
Figure 4.1: Graph of Epsom Salt in Different Type of Solvents Versus Temperature
According to Figure 4.1, it showed than the solubility of Epsom salt in the solvents
were increased proportionally with its temperature. This was because the kinetic energy of the
solvent molecules increased accordingly with the temperature which allowed the molecules to
be more effectively broke apart the solute molecules that were held together by intermolecular
attractions. Besides, the water solvent had the highest solubility, followed by ethanol and
acetone. Solubility depended on the polarity of the compound and interaction between solute
and solvent molecules. The molecule of similar structure and polarity will mix well and soluble
in each other (Recrystallization and Melting Points, n.d). Hence, the stronger the attraction
between solute and solvent molecules, the higher the solubility. Epsom salt was a polar
molecule with unshared pairs of electrons between sulphate and oxygen atoms. It had a strong
attractive that allowed to dissolve in polar solvent only. Water was a polar solvent with
hydrogen bonding whereas ethanol was a very polar molecule due to its hydroxyl (OH) group
with high electronegativity of oxygen which allowing hydrogen bonding to take place with
other molecules. However, Epsom salt had higher solubility in water because both of water and
salt were more compatible as they can form ionic compounds. The Epsom salt was less soluble
in acetone because the acetone was significantly less polar than water and ethanol. Hence, the
Epsom salt had the lowest solubility in acetone solvent.
A linear form of Van’t Hoff equation was showed in the following (Standard, 2015):
∆Go = -RT ln Keq
ln Keq = -∆Go/RT
∆Go = ∆Ho – T ∆So
∆ 𝐻𝑜 ∆ 𝑆𝑜
ln Keq = - +
𝑅𝑇 𝑅
1 ∆ 𝐻𝑜 ∆ 𝑆𝑜
where y = ln Keq, x = 𝑇 , m = - 𝑅
,c= , R = 8.314 J/mol.K
𝑅
The Keq was calculated using the following formula:
𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑆𝑎𝑙𝑡 (𝑔)

𝑔
𝑀𝑊 𝑜𝑓 𝐸𝑝𝑠𝑜𝑚 𝑆𝑎𝑙𝑡 ( )
𝑚𝑜𝑙
Keq = 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑆𝑎𝑙𝑡 (𝑔) 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑆𝑜𝑙𝑣𝑒𝑛𝑡 (𝑔)
𝑔 + 𝑔
𝑀𝑊 𝑜𝑓 𝐸𝑝𝑠𝑜𝑚 𝑆𝑎𝑙𝑡 ( ) 𝑀𝑊 𝑜𝑓 𝑆𝑜𝑙𝑣𝑒𝑛𝑡 ( )
𝑚𝑜𝑙 𝑚𝑜𝑙
According to Perry Chemical Handbook, the molecular weight of acetone, ethanol,
water and Epsom salt were 58.08 g/mol, 92.14 g/mol, 18.02 g/mol and 120.36 g/mol. Since 1
mL of water weighed 1 g under standard condition, 1 mL of any sample was assumed equal to
1 g (Dilution Theory and Problems, n.d.).
Table 4.2: Data for Different Solvents and Temperatures Used in Van’t Hoff Equation
Solvent Temperature, T (K) 1/T (K-1) Keq (mole/mole) ln Keq
Acetone 303 0.0033 0.0152 -4.1865
313 0.0032 0.0180 -4.0174
323 0.0031 0.0254 -3.6730
Ethanol 303 0.0033 0.2198 -1.5150
313 0.0032 0.2974 -1.2127
323 0.0031 0.3377 -1.0856
Water 303 0.0033 0.1187 -2.1312
313 0.0032 0.1323 -2.0227
323 0.0031 0.1527 -1.8793
1/T versus ln Keq

1/T (K-1)
0
0.00305 0.0031 0.00315 0.0032 0.00325 0.0033 0.00335
-0.5
-1
y = -2147x + 5.5993
-1.5
y = -1259.5x + 2.0193
-2
ln Keq
-2.5
-3
-3.5
y = -2567.5x + 4.257
-4
-4.5
Acetone Ethanol Water Linear (Acetone) Linear (Ethanol) Linear (Water)
Figure 4.2: Graph of 1/T Versus ln Keq for Different Solvents

Table 4.3: Data of Dissolution Enthalpy and Entropy for Different Solvents
Solvent Slope Intercept Dissolution Dissolution
Enthalpy, ∆𝑯 Entropy, ∆𝑺
(J/mol) (J/mol.K)
Acetone -2567.5 4.2570 21346.195 35.3927
Ethanol -2147.0 5.5993 17850.158 46.5526
Water -1259.5 2.0193 10471.483 16.7885
The Van’t Hoff Equation was derived from Gibbs-Helmholtz equation and provided
the information about the temperature dependence of the equilibrium constant. Based on Table
4.3, the positive value of the dissolution enthalpy indicated the dissolution process of the
Epsom salt in various solvents was an endothermic reaction in which the heat was absorbed by
the system due to the products of the reaction having a greater enthalpy than reactants. For
positive value of dissolution entropy, it implied an increased in disorder in which all
spontaneous changes occurred with an increase in entropy of the universe. Acetone had the
highest dissolution enthalpy of 21346.195 J/mol which indicated that the reaction absorbed a
lot of heat for the reaction, followed by ethanol (17850.158 J/mol) and water (10471.483 J/mol).
From Figure 4.2, the Van’t Hoff plot showed a negative slope which indicated that the
dissolution was an endothermic reaction for all different type of solvents. Based on Le
Chatelier’s Principle, it predicted that if the reaction temperature increased, the system will
shift to the right for the additional heat and lead to an increase in products and a decrease in
reactants (Standard, 2015). Thus, more Epsom salt will be dissolved and resulted an increase
in solubility.
4.2 Different Type of Crystal

Solvent: Distilled Water
Temperature: 50 oC
Volume: 10 mL
Table 4.4: Experimental Results of Sugar, Copper Sulphate and Epsom Salt in Distilled Water
Component Empty Crucible Wet Weight Dry Weight Solubility
Weight (g) (g) (g)
Sugar 31.5165 35.2946 32.4934 0.0977

Copper Sulphate 31.5251 37.1038 32.3690 0.0844
Epsom Salt 30.9432 38.0157 32.6583 0.1715
Table 4.5: Solid Appearance of Sugar, Copper Sulphate and Epsom Salt Before and After
Crystallization in Distilled Water
Component Solid Appearance
Before After
Sugar
Copper Sulphate
Epsom Salt
According to Table 4.5, based on the picture of sugar solution after crystallization, it
showed a lattice structure of monoclinic. The sugar crystal looked clear and sparkling. For
copper sulphate, the crystal formed was a bright blue crystal. It appeared in short prismatic
form and in thick tabular translucent crystals. Its lattice structure arrangement was triclinic with
molecular formula CuSO4.5H2O (Lide, 2003). The crystal was known as copper (II) sulphate
pentahydrate. For Epsom salt, it showed fibrous structure in white colour. The crystal formed
was called epsomite with molecular formula MgSO4.7H2O. Its lattice structure was
orthorhombic (Lide, 2003).
4.3 Crash Cooling Versus Natural Cooling Recrystallization

Table 4.6: Temperature of Epsom Salt to Crystallize Under Ice Bath and Room Temperature
Time Ice Batch Cooling Natural Cooling
(min)
Temperature Observation Temperature Observation
0 50 - 50 -
1 44 - 49 -
2 41 - 47 -
3 38 - 46 -
4 35 - 45 -
5 32 - 44 -
6 29 - 42 -
7 25 - 42 -
8 23 - 41 -
9 20 - 40 -
10 18 - 39 -
11 16 - 39 -
12 14 - 38 -
13 13 - 38 -
14 12 - 38 -
15 11 Crystallize 37 - (Nothing)
Figure 4.3: Ice Bath Cooling Figure 4.4: Natural Cooling
Crystallization was a process where solid particles were formed from a homogeneous
phase. The solution was saturated and usually cooled until the solute concentration became
larger than its solubility at given temperature. The crystals formed typically had flat faces and
sharp corner (Geankoplis, 2003). Based on Table 4.6, it was noticed that the crystal was formed
at 15th minutes for the ice bath cooling whereas no crystal was found during natural cooling.
Figure 4.3 and Figure 4.4 showed the observation at the end of the experiment. There was a
large amount of crystal formed during ice bath cooling. This was because the ice bath promoted
the crystal growth by lowering the temperature quickly and dramatically.
5.0 CONCLUSION AND RECOMMENDATION
In a nutshell, when the temperature increased, the solubility of the solute in the solvent
also increased due to higher kinetic energy gained by the solvent molecules to break apart the
solutes which were held by intermolecular attractions. Next, water solvent had the highest
solubility of Epsom salt (1.204 g/mL), followed by ethanol (1.018 g/mL) and acetone (0.900
g/mL) at high temperature of 50oC. This phenomenon occurred because Epsom salt had higher
solubility in water as both of water and salt were more compatible to form ionic compounds.
For instance, Epsom salt was less soluble in acetone because it was significantly less polar than
water and ethanol. Besides, the Van’t Hoff plot showed a negative slope which indicated that
this experiment was an endothermic reaction for all different type of solvents. Acetone had the
highest dissolution enthalpy of Epsom salt (21346.195 J/mol) which implied that the reaction
absorbed massive heat for the reaction, followed by ethanol (17850.158 J/mol) and water
(10471.483 J/mol). The dissolution entropy of Epsom salt was found to be 35.3927 J/mol.K,
46.5526 J/mol.K and 16.7885 J/mol.K for acetone, ethanol and water respectively. Moreover,
based on the observation, the crystal shape of sugar, copper sulphate and Epsom salt in distilled
water were appeared in monoclinic, triclinic and orthorhombic lattice structure respectively.
According to the result of the recrystallization of Epsom salt using ice batch cooling and natural
cooling crystallization, it was noticed that large amount of crystal was formed at 15th onwards
during ice bath cooling as the cold condition promoted the crystal growth whereas there was
no crystal forming during natural cooling.
For the recommendation, the Epsom salt must be added slowly to the solvent and the
solution must be stirred thoroughly until the salt solute was just excess in the solvent for the
accuracy of the value of solubility. In addition, the Epsom salt in the solvent must be stirred at
higher speed to minimize the mass transfer resistance between the salt and solvent when
determining its solubility. Lastly, advance equipment like Field Emission Scanning Electron
Microscopy (FE-SEM) should be used to have a better study on the structure of the crystal
formed.
6.0 REFERENCES
Dilution Theory and Problems. (n.d.). Retrieved from

http://www.biofsu.edu/courses/mcb4403L/dilution.pdf
Geankoplis, C.J. (2003 (4th Edition)). Transport Processes and Separation Process Principles.
New Jersey: Pearson Education Inc.
Hallas N.J. (2011, February 2). Crystallization. doi:10.1615/AtoZ.c.crystallization
L. Yu, & S.M. Reutzel-Edens. (2003). Crystallation| absic Principle. Encyclopedia of Food
Sciences and Nutrition , 1697-1702.
Lide, D.R. (2003). CRC Handbook of Chemistry and Physics. 84 th Edition. CRC Press.
Recrystallization and Melting Points. (n.d.). Retrieved from

http://courses.chem.psu.edu/chem36/Experiments/recrstal.pdf
Standard, J. M. (2015, March 27). The Van’t Hoff Equation. Retrieved from
http://chemistry.illnuisstate.edu/standard/che360/handouts/360vanthoff.pdf
Zurich. (2008). Process Engineering Laboratory II Crystalizlation. Spring.

7.0 APPENDICES
Nine crucibles were placed in the

furnace for drying overnight. The
crucibles were wrapped with
aluminium foil.
The shapes of crystal

formed were observed.
UNIT OPERATION LAB
(BKF3731)
Title of Experiment : Thin Film Evaporation
Date of Experiment : 17 April 2018
List of Students :
Name Student’s ID
Group No. :3
Section : 02
Marks :
Title of Experiment : Thin Film Evaporation

TABLE OF CONTENT
No. Title Page
1.0 Abstract 1
2.0 Introduction 2
3.0 Methodology 3
6.0 References 10
7.0 Appendices 11
1.0 ABSTRACT
Thin film evaporation unit was a complete evaporation system including feed input,
heating and vacuum generation for continuous plant operation. The objective of this experiment
was to demonstrate the evaporation of ethanol – water mixture and to determine the effect of
heating temperature and vacuum pressure on the evaporation rate. The experiment was started
with the preparation of calibration curve for a set of mixtures containing ethanol and water
versus refractive index (RI) by manipulating the concentration of ethanol at 0%, 25%, 50%,
75%, 90% and 100%. Then, a mixture of ethanol and water at composition of 60:40 was feed
into the thin film evaporation unit. The heating equipment thermostat T1 was set to 80 oC and
the vacuum controller PIC-1 was fixed at 250 mbar. The system was allowed to reach the
setting value and then the feed metering pump was started. The equipment was running for 7
minutes and the distillate and bottom product flow rates were measured. The product from both
distillate and bottom product vessels B2 and B3 were collected and analysed to determine its
refractive index and composition. The experiment was repeated by increasing the heating
thermostat up to 85 oC and 90 oC at fixed vacuum pressure of 250 mbar. The experiment also
repeated by using different vacuum pressure of 350 mbar, 300 mbar and 250 mbar at constant
heating temperature of 90 oC. The calibration curve illustrated that the higher the percentage
of ethanol in water, the higher the refractive index (RI). The experimental result showed that
the flow rate and composition of ethanol in distillate increased when increasing the heating
temperature due to higher kinetic energy gained by the ethanol-water mixture and the lower
boiling point of the ethanol compared to water. Hence, the evaporation rate of ethanol was
increasing which eventually resulted in a high flow rate and composition of ethanol in distillate.
However, the flow rate and composition of ethanol in distillate decreased when increasing the
vacuum pressure due to high boiling point of ethanol-water mixture resulted at high vacuum
pressure and this had cause the difficulty for the ethanol to evaporate as it required enough high
kinetic energy to reach its boiling point. Thus, the evaporation rate of ethanol was decreasing
which eventually resulted in a low flow rate and composition of ethanol in distillate. Thin film
evaporator was suggested to be operated at a lower vacuum pressure to improve evaporator
efficiency.
2.0 INTRODUCTION
Thin film evaporator provided short residence time and open, low pressure drop
configuration, allowing continuous, reliable processing of many heat sensitive, viscous, or
fouling materials without product degradation. The thin film evaporation unit was a complete
evaporation system including feed input, heating and vacuum generation for continuous plant
operation. The unit was designed to evaporate materials in the pressure range of atmospheric
down to 8 mbar. The lower the pressure, the lower the temperature required to effect
evaporation thus lowering the chances of damaging the product. The thin film evaporator
adopted a rotating film system where molecules were continuously evaporating from a film
which was spread by a rotating wiper (Thin Film/ Wiped Film Evaporator, 2017).
Thin film evaporators quickly separated more volatile from less volatile components
using indirect heat transfer and mechanical agitation of a flowing product film under controlled
conditions (Thin Film/ Wiped Film Evaporator, 2017). The rotor was to stabilize the liquid film
on the heating surface at high evaporation rates. On the one hand, evaporation in the area of
nucleate boiling was possible without ruptures of the film. Besides, the liquid film was pressed
against the heating surface by the centrifugal force. This avoided the adverse evaporation mode,
in which a vapour layer with insulating effect was formed under the liquid film. Therefore, due
to the functional principle extremely high specific evaporation rates were achievable in thin
film evaporators (SMS , 2017).
The advantages of thin film evaporators compared to other evaporator types were the
reliable processing of viscous, fouling and soiled liquids and the low hold-up with minimal
losses in case of product changes. The application of thin film evaporator was for distillation,
separation, deodorization and continuous processing (SMS , 2017).
3.0 METHODOLOGY
Materials: Ethanol and Water
Apparatus: BP215 Thin Film Evaporator, Stop Watch, Beakers, Refractometer, Cooling
Water Supply, and Measuring Cylinder
3.1 Preparation of Calibration Curve
Two sets of standard mixtures about 10 mL in total containing ethanol and water within a specified
range of composition of ethanol, which were 0%, 25%, 50%, 75%, 90% and 100% were prepared.
Refractive index (RI) for each mixture was determined by using a refractometer.
3.2 Experimental Procedure
5 L of ethanol-water mixture at a composition of 60:40 v/v was prepared.
Equipment parts and function of the evaporator unit were identified.
The heating equipment thermostat T1 was set to 80 oC and the vacuum controller PIC-1 was
fixed at 250 mbar.
The system was allowed to reach the setting value and then the feed metering pump was started.
The equipment was running for 7 minutes.
The distillate and bottom product flow rates were measured.
The product from both distillate and bottom product vessels B2 and B3 were collected. The
collected liquid was analysed to determine its refractive index and composition.
The experiment was repeated by increasing the heating thermostat up to 85 oC and 90 oC at fixed
vacuum pressure of 250 mbar.
The experiment also repeated by using different vacuum pressure of 350 mbar, 300 mbar and
250 mbar at constant heating temperature of 90 oC.
4.0 RESULTS AND DISCUSSION
4.1 Data Collection for Calibration Curve
Table 4.1: Calibration Curve Data
Standard Concentration (mol %) Refractive Index (RI)
Set 1 Set 2 Average
1 0 1.3292 1.3292 1.3292
2 25 1.3387 1.3381 1.3384
3 50 1.3473 1.3469 1.3471
4 75 1.3532 1.3528 1.3530
5 90 1.3570 1.3576 1.3573
6 100 1.3634 1.3648 1.3641
Refractive Index vs Concentration

1.37
1.365
Refractive Index
1.36
1.355
1.35
y = 0.0003x + 1.3295
1.345 R² = 0.9934
1.34
1.335
1.33
1.325
0 20 40 60 80 100 120
Concentration , mol%
Figure 4.1: Calibration Curve of Refractive Index versus Concentration of Ethanol in Water
Figure 4.1 showed the calibration curve of refractive index versus concentration of
ethanol in water, where the slope = 0.0003and y-intercept = 1.3295. The equation that related
refractive index to the composition was:
Refractive Index = 0.0003(concentration((mol%)) + 1.3295
From the calibration curve above, it showed that the refractive index increased with the
concentration of ethanol. The higher the concentration of ethanol, the higher the value of
refractive index and vice versa. From the data, the refractive index of pure ethanol and pure
water are 1.3641 and 1.3292 respectively.
4.2 Effect of Temperature at Constant Pressure of 250 mbar
Table 4.2: Flow Rate for Distillate and Bottom at Constant Pressure of 250 mbar
Run Heating Vacuum Distillate Bottom
Temp. Pressure Volume Time Flow Rate Volume Time Flow Rate
(oC) (mbar) (mL) (min) (mL/min) (mL) (min) (mL/min)
1 80 250 50 7 7.1429 200 7 28.5714

2 85 250 80 7 11.4286 170 7 24.2857
3 90 250 110 7 15.7143 150 7 21.4286
Table 4.3: Composition for Distillate and Bottom at Constant Pressure of 250 mbar
Temp. Pressure RI Composition RI Composition
(oC) (mbar)
1 80 250 1.3515 0.7333 1.3435 0.4667

2 85 250 1.3540 0.8167 1.3375 0.2667
3 90 250 1.3572 0.9233 1.3330 0.1167
Flow Rate of Distillate and Bottom versus Temperature at

Constant Pressure
30
25
Flow Rate (mL/min)
20
15
10
0
78 80 82 84 86 88 90 92
Temperature (oC)
Distillate Bottom
Figure 4.2: Graph of Flow Rate of Distillate and Bottom versus Temperature
Composition of Ethanol versus Temperature at Constant
Pressure
1
0.9
Composition of Ethanol
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
78 80 82 84 86 88 90 92
Temperature (oC)
Distillate Bottom
Figure 4.3: Graph of Composition of Ethanol versus Temperature
Figure 4.2 showed the relationship between flow rate of distillate and bottom with the
temperature. When the temperature increased, the flow rate of distillate was increasing whereas
the flow rate of bottom was decreasing. According to Figure 4.3, it can be concluded that when
the temperature of ethanol-water mixture increased, the composition of ethanol in the distillate
and bottom were increased and decreased respectively. The reason why these two phenomenon
occurred was because the molecules of the mixture possessed a high amount of kinetic energy
at high temperature which made the mixture to be evaporated easily under high temperature
(Y. Miyazaki et al, 2006). For instance, ethanol was more volatile when compared to water due
to its low boiling point which eventually caused high amount of ethanol to be evaporated in
distillate. As more of the ethanol was being evaporated in distillate, this lead to the lesser
composition of ethanol in the bottom. As a result, increasing in flow rate and composition of
ethanol resulted in the distillate whereas decreasing in flow rate and composition of ethanol
resulted in the bottom when the heating temperature of the thin film evaporator was increased.
4.3 Effect of Pressure at Constant Temperature of 90 oC
Table 4.4: Flow Rate for Distillate and Bottom at Constant Temperature of 90 oC
Temp. Pressure Volume Time Flow Rate Volume Time Flow Rate
(oC) (mbar) (mL) (min) (mL/min) (mL) (min) (mL/min)
1 90 350 30 7 4.2857 375 7 53.5714

2 90 300 80 7 11.4286 250 7 35.7143
3 90 250 140 7 20.0000 150 7 21.4286
Table 4.5: Composition for Distillate and Bottom at Constant Temperature of 90 oC

Temp. Pressure RI Composition RI Composition
(oC) (mbar)
1 90 350 1.3566 0.9033 1.3429 0.4467
2 90 300 1.3570 0.9167 1.3395 0.3333
3 90 250 1.3575 0.9333 1.3335 0.1333
Flow Rate of Distillate and Bottom versus Pressure at Constant

Temperature
60
50
Flow Rate (mL/min)
40
30
20
10
0
220 240 260 280 300 320 340 360
Pressure (mbar)
Distillate Bottom
Figure 4.4: Graph of Flow Rate of Distillate and Bottom versus Pressure
Composition of Ethanol versus Pressure at Constant
Temperature
1
0.9
Composition of Ethanol
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
220 240 260 280 300 320 340 360
Pressure (mbar)
Distillate Botton
Figure 4.5: Graph of Composition of Ethanol versus Pressure
Based on Figure 4.4, when the vaccum pressure increased, the flow rate of distillate
was decreasing whereas the flow rate of bottom was increasing. From Figure 4.5, it can be
summarised that when the vacuum pressure of ethanol-water mixture increased, the
composition of ethanol in the distillate and bottom were decreased and increased respectively.
These two phenomenon occurred was because when the vacuum pressure was increased, the
boiling temperature of the ethanol-water mixture will be increased too in which this will
decrease the evaporation rate of ethanol as it had to achieve enough high kinetic energy to reach
it high boiling point. Consequently, less amount of ethanol will be evaporated in distillate and
this lead to the increased amount of ethanol resulted in the bottom. Thus, decreasing in flow
rate and composition of ethanol resulted in the distillate whereas increasing in flow rate and
composition of ethanol resulted in the bottom when the vacuum pressure of the thin film
evaporator was increased.
In a nutshell, from the calibration curve, the higher the percentage of ethanol in water,
the higher the refractive index (RI). From the experimental result, when the heating temperature
was increased from 80 oC to 90 oC, the flow rate in the distillate increased from 7.1429 mL/min
to 15.7143 mL/min. The ethanol composition in the distillate stream also increased from 0.7333
to 0.9233 because of the elevation in heating temperature. This phenomenon happened due to
higher kinetic energy gained by the ethanol-water mixture and the lower boiling point of the
ethanol compared to water. Hence, the evaporation rate of ethanol was increasing which
eventually resulted in a high flow rate and composition of ethanol in distillate. However, when
the vacuum pressure was increased from 250 mbar to 350 mbar, the flow rate in distillate
decreased from 20.0000 mL/min to 4.2857 mL/min. The ethanol composition in the distillate
stream also decreased from 0.9333 to 0.9033 because of the elevation in vacuum pressure. This
situation occurred due to high boiling point of ethanol-water mixture resulted at high vacuum
pressure and this had cause the difficulty for the ethanol to evaporate as it required enough high
kinetic energy to reach its boiling point. Thus, the evaporation rate of ethanol was decreasing
which eventually resulted in a low flow rate and composition of ethanol in distillate.
For the recommendation, the thin film evaporator should be operated at a lower vacuum
pressure to improve the efficiency of the evaporator. Besides, the bottom and distillate vessel
were opened before started the experiment to make sure that there was no excess product left
in it from the previous experiment as the contamination may occur which eventually will affect
the reading of refractive index. In addition, the point of refractometer must be submerged
completely with the solution when measuring the refractive index and it must be rinsed with
distilled water after every use.
6.0 REFERENCES
SMS. (2017). Thin Film Evaporator: The evaporator for demanding applications. Retrieved
from http://www.sms-vt.com/technologies/evaporation-technology/thin-film-evaporator/
Thin Film / Wiped Film Evaporator. (2017). Retrieved from

https://lcicorp.com/thin_film_evaporation/thin_film_wiped_film_evaporator
Y. Miyazaki, Y. Onuki, S. Yakou, K. Takuyama. (2006). Effect of temperature-increase rate

on drug release characteristics of dextran microspheres prepared by emulsion solvent
evaporation process, International Journal of Pharmaceutics, 144-151.
7.0 APPENDICES
Overview process of thin film evaporator.
The solution was collected at the distillate and bottom vessel.

UNIT OPERATION LAB
(BKF3731)
Title of Experiment : Short Path Distillation
Date of Experiment : 27 February 2018
List of Students :
Name Student’s ID
Group No. :3
Section : 02
Marks :
Subject Code : BKF3731 Date Submitted: 6 March 2018
Title of Experiment : Short Path Distillation

TABLE OF CONTENT
No. Title Page
1.0 Abstract 1
2.0 Introduction 2
3.0 Methodology 3
6.0 References 10
7.0 Appendices 11
1.0 ABSTRACT
Short path distillation was a thermal separation process for thermal sensitive products.
The objective of this experiment was to study the effect of temperature and stirrer speed on the
efficiency of ethylene glycol-water separation in a short path distillation. In this experiment, a
homogenous mixture of ethylene glycol and water with a ratio of 5:5 at total of 2 L was
prepared by mixing 1 L of ethylene glycol with 1 L of water and fed into the short path
distillation unit. The experiment was first carried out by varying the evaporator temperature at
70°C, 80°C, 90°C and 100°C with constant stirrer speed of 15 rpm. Next, the experiment was
repeated by manipulating the stirrer speed at 50 rpm, 100 rpm, 150 rpm and 200 rpm with
constant temperature of 85°C to study its effect on separation efficiency. The volume of the
distillate and concentrate were measured and recorded at every 10 minutes. The refractive
index for both distillate and bottom were then be measured by using refractometer. The data
was tabulated, and the separation efficiency was calculated. The result showed both distillate
and concentrate volume increased as temperature and stirrer speed were increased. The
separation efficiency for temperature at 70°C, 80°C, 90°C and 100°C were 99.05%, 99.27%,
99.43% and 99.45% respectively. In the meanwhile, the separation efficiency for stirrer speed
at 50 rpm, 100 rpm, 150 rpm and 200 rpm were 99.07%, 99.13%, 99.15% and 99.23%
respectively. From the result, it could be clearly seen that the increase of evaporator
temperature and stirrer speed will improve the separation efficiency of short path distillation
due to the molecules of the ethylene glycol-water mixture gained higher kinetic energy. For
the recommendation, the ice should be added to cold trap from time to time to maintain its
temperature. This was to ensure that all vapours except the permanent gases were condensed
into liquids, trapping them in the container and keeping them from reaching the vacuum pump.
This can prevent the vapours from entering the vacuum pump which they would condense and
contaminate the pump.
2.0 INTRODUCTION
Short path distillation is a distillation technique that involves the distillate travelling a
short distance, often only a few centimetres, and is normally done at reduced pressure. The
vapour stream travels a "short path" directly to the condenser which is located within the
evaporator chamber. Since the vapour stream is immediate condensed, the short path
distillation process precludes the vapour from forming vapour pressure. This allows ultimate
pressures of 0.001 mbar to be attained. Short residence time and low evaporation temperature
will cause a minimum thermal stress to the distilled product. This also allows heat sensitive
materials to undergo purification at much lower temperatures preventing degradation. A short
path ensures that little compound is lost on the sides of the apparatus. Typical applications are
high molecular organic compounds particularly from the fields of chemistry, pharmaceutical
and food industry.
Short path distillation is a continuous separation process working under vacuum
conditions. Evaporation takes place from a heated wiped film. Caused by the pressure
drop between the place of vaporization and the vacuum system the operating pressure in typical
wiped film evaporators with external condenser is limited to some millibars. The considerably
lower pressure in the short path evaporator is obtained by the short distance for the vapors on
theirway from the evaporator surface to the condenser. In addition, the cross-section area of
flow is equal to the evaporator surface, so that there is only a minor pressure drop between
evaporator and condense.
Separation of components from a liquid mixture via distillation depends on the
differences in boiling point of the individual components. Also, depending on the
concentrations of the component present, the liquid mixture will have different boiling point
characteristics. Therefore, distillation processes depend on the vapour pressure characteristics
of liquid mixtures. The vapour pressure of a liquid at a particular temperature is the pressure
exerted by molecules leaving and entering the liquid surface. Here are some important points
regarding vapour pressure: energy input raises vapour pressure, vapour pressure is related to
boiling, a liquid is say to “boil” when its vapour pressure is equals the surrounding pressure.
The ease with which a liquid boil depends on its volatility liquids with high pressure will boil
at lower temperature, the vapour pressure and hence the boiling point of the liquid mixture
depends on the relative amounts of component in mixture. Distillation occurs because of the
difference in the volatility of the component in the liquid mixture. The separation efficiency
denotes by:
𝐶𝑜𝑛𝑑𝑒𝑛𝑠𝑎𝑡𝑒 𝑉𝑜𝑙𝑢𝑚𝑒
Separation efficiency = x 100%
𝐹𝑒𝑒𝑑 𝑉𝑜𝑙𝑢𝑚𝑒
3.0 METHODOLOGY
Equipment / Apparatus / Material: 1. Short Path Distillation Unit
2. Ethylene Glycol-Water Mixture
3. EG-Water refractometer
Experimental Procedures:
The ethylene glycol and water with a ratio of 5:5 were mixed at total of 2 L in a
beaker. Then the mixture was stirred homogeneously.
The feed mixture was preheated to 60oC on heating plate and connected to the
peristaltic feed pump.
All valves were initially closed except the valves HV04, HV05, HV11 and
HV12. The cold trap was filled with dry ice.
The main power supply was switched on at the control panel.
The thermostat, chiller and vacuum pump pressure were set at 70oC, 12oC and
200 mbar. The pressure was manually maintained throughout the experiment.
Once the chiller temperature and thermostat temperature had reached the set
points, the feed pump was turned on and set to 10 rpm and then stirrer was
turned on.
Every set of experiments was run for 10 minutes and the volume of distillate
from V-104 and volume of concentrate from V-105-107 were recorded. The
refractive index (RI) for distillate and bottom were measured.
The experiment was repeated with different stirrer speeds and different
temperatures.
The operating procedure was followed to shut down the equipment.

4.1 Data Collection
4.1.1 Effect of Evaporator Temperature
Vacuum Pressure, PT-200 : 200 mbar
Stirrer Speed, M-500 : 15 rpm
Feed Flow Rate : 28.80 mL/min
Contact Time : 10 minutes
Ethylene Glycol – Water Ratio : 5:5
Table 4.1: Effect of Evaporator Temperature on Separation Efficiency
Distillate Volume (mL) Concentrate Volume (mL)

Separation
Run Temp (°C) Vol, mL %EG Vol, mL %EG Efficiency (%)
1 70 8 13.2 270 40.6 99.05
2 80 10 8.8 275 43.7 99.27
3 90 11 6.8 280 46.2 99.43
4 100 13 5.6 285 46.4 99.45
4.1.2 Effect of Stirrer Speed

Vacuum Pressure, PT-200 : 200 mbar
Evaporator Temperature, TT-100 : 85oC
Feed Flow Rate : 25.75 mL/min
Contact Time : 10 minutes
Ethylene Glycol – Water Ratio : 5:5
Table 4.2: Effect of Stirrer Speed on Separation Efficiency
Distillate Volume (mL) Concentrate Volume (mL)

Separation
Run Stirrer Speed (rpm) Vol, mL %EG Vol,mL %EG Efficiency (%)
1 50 11 7.4 215 40.2 99.07
2 100 13 6.6 220 44.3 99.13
3 150 17 6 250 47.8 99.15
4 200 19 5.6 285 48 99.23
4.2 Calculation of Feed Flow Rate
The feed flow rate of the reactants can be calculated by using the formula as shown below:
(𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐷𝑖𝑠𝑡𝑖𝑙𝑙𝑎𝑡𝑒)+(𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑒)
Feed flow rate (mL/min) = 10 𝑚𝑖𝑛𝑢𝑡𝑒𝑠

Table 4.3: Feed Flow Rate for Evaporator Temperature Effect
Volume of Distillate (mL) Volume of concentrate (mL) Feed flow rate (mL/min)
8 270 27.80
10 275 28.50
11 280 29.10
13 285 29.80
𝟐𝟕.𝟖𝟎 +𝟐𝟖.𝟓𝟎 +𝟐𝟗.𝟏𝟎 +𝟐𝟗.𝟖𝟎

Average feed flow rate = = 28.80 mL/min
𝟒
4.2.2 Effect of Stirrer Speed

Table 4.4: Feed Flow Rate for Stirrer Speed Effect
Volume of Distillate (mL) Volume of concentrate (mL) Feed flow rate (mL/min)
11 215 22.60
13 220 23.30
17 250 26.70
19 285 30.40
𝟐𝟐.𝟔𝟎 +𝟐𝟑.𝟑𝟎 +𝟐𝟔.𝟕𝟎 +𝟑𝟎.𝟒𝟎

Average feed flow rate = = 25.75 mL/min
𝟒
4.3 Calculation of Separation Efficiency
Separation efficiency for both effect of evaporator temperature and stirrer speed can be
calculated by using the formula as shown below:
Separation efficiency =
(𝑣𝑜𝑙𝑢𝑚𝑒 𝑥 𝑐𝑜𝑚𝑝. 𝑜𝑓 𝑒𝑡ℎ𝑦𝑙𝑒𝑛𝑒 𝑔𝑙𝑦𝑐𝑜𝑙) 𝑖𝑛 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑒
(𝑣𝑜𝑙𝑢𝑚𝑒 𝑥 𝑐𝑜𝑚𝑝.𝑜𝑓 𝑒𝑡ℎ𝑦𝑙𝑒𝑛𝑒 𝑔𝑙𝑦𝑐𝑜𝑙) 𝑖𝑛 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑒 + (𝑣𝑜𝑙𝑢𝑚𝑒 𝑥 𝑐𝑜𝑚𝑝.𝑜𝑓 𝑒𝑡ℎ𝑦𝑙𝑒𝑛𝑒 𝑔𝑙𝑦𝑐𝑜𝑙) 𝑖𝑛 𝑑𝑖𝑠𝑡𝑖𝑙𝑙𝑎𝑡𝑒
𝑥 100%
(Retrieved from: https://www.academia.edu/8885393/Exp3_shortcut_distillation_)

For an example, at 70oC, the separation efficiency can be calculated as follow:
270 𝑥 0.406
Separation efficiency = (270 𝑥 0.406)+(8 𝑥 0.132) x 100% = 99.05%

Table 4.5: Separation Efficiency for Evaporator Temperature Effect
Temp (°C) Separation Efficiency (%)
70 99.05
80 99.27
90 99.43
100 99.45
Effect of Evaporator Temperature on the Separation Efficiency

99.60
Separation Efficiency, %
99.50
99.40
99.30
99.20
99.10
99.00
65 70 75 80 85 90 95 100 105
Temperature,°C
Figure 4.1: Graph of Separation Efficiency versus Temperature

Figure 4.1 showed the relationship between the evaporator temperature and the
separation efficiency with the stirrer speed set at constant speed of 15 rpm. According to Table
4.3, when the temperature was increasing from 70oC to 100oC, the separation efficiency was
increasing from 99.05% to 99.45%. Based on the result, it can be concluded that the separation
efficiency was proportional to the evaporator temperature as when the evaporator temperature
was increasing, the separation efficiency was increasing too. This was because the boiling was
achieved faster at high temperature with more heat energy supply. At a higher temperature, the
molecules of the mixture gained higher kinetic energy and this lead to higher collision per unit
time between the reactant particles. (Moller et al, 2002) Thus, the effective collision frequency
was increased which result in the increased of the separation efficiency in short path distillation.
In addition, short path distillation will also be affected by the change in pressure. Short
path distillation is a distillation technique that usually carried out at reduced pressure. (Albers
& Alzenau-Horstein, 2012) Thus, when the pressure was increased, the performance of the
short path distillation unit will be lower as the mixture required a higher evaporator temperature
to be separated. The higher the pressure, the higher the temperature needed for the mixture to
reach boiling point. Therefore, the pressure need to be maintain constant throughout the
experiment when the stirring speed and evaporator temperature were manipulated to get an
accurate result for the separation efficiency of ethylene glycol-water in short path distillation.
4.3.2 Effect of Stirrer Speed on the Separation Efficiency

Table 4.6: Separation Efficiency for Stirrer Speed Effect
Stirrer Speed (rpm) Separation Efficiency (%)

50 99.07
100 99.13
150 99.15
200 99.23
Effect of Stirrer Speed on the Separation Efficiency

99.24
99.22
99.20
Separation Efficiency, %
99.18
99.16
99.14
99.12
99.10
99.08
99.06
99.04
0 50 100 150 200 250
Stirrer Speed, rpm
Figure 4.2: Graph of Separation Efficiency versus Stirrer Speed

Based on Table 4.4, by setting the evaporator temperature at constant at 85oC, the higher
the stirrer speed, the higher the separation efficiency of the short path distillation. From the
Figure 4.2, it can be implied that the separation efficiency was directly proportional to the
stirrer speed as it showed a linearly increasing best fit line. When the stirrer speed was
increasing from 50 rpm to 250 rpm, the separation efficiency was increasing from 99.07% to
99.23%. It was noted that the percentage of ethylene glycol in the distillate was gradually
decreased from 7.4% to 5.6% whereas the percentage of ethylene glycol in the concentrate was
gradually increased from 40.2% to 48% upon the increased of the stirrer speed. The reason was
because the water had the lower boiling point as compared to ethylene glycol. As a result, this
caused the water to dominate the distillate whereas the concentrate mainly comprised of
ethylene glycol. Besides, the percentage of ethylene glycol in the distillate was decreasing upon
the increasing of the stirrer speed as the molecules of the mixture gained higher kinetic energy
which eventually caused the water (light component) to be easily evaporated in a faster rate.
In a nutshell, both evaporator temperature and stirrer speed will affect the separation
efficiency of the short path distillation. When the evaporator temperature increased from 70oC
to 100oC, the separation efficiency increased from 99.05% to 99.45% due to the higher kinetic
energy supplied at higher temperature that eventually increase the effective collision frequency
of the reactant particles. Meanwhile, when the stirrer speed increased from 50 rpm to 200 rpm,
the separation efficiency increased from 99.07% to 99.23% due to the molecules of reactants
gained higher kinetic energy which eventually caused more water (light component) to be
evaporated at a faster rate that resulted in higher composition of ethylene glycol in the
concentrate.
For the recommendation, the refractory meter must be rinsed with distilled water each
time before it was used to measure the percentage of ethylene glycol to prevent inaccurate
reading. Moreover, the cold trap must be trapped up with dry ice from time to time to create a
vacuum space for the short path distillation. Furthermore, the ethylene glycol mixture must be
handled with care as it was quite corrosive to human body. Besides, the temperature of the feed
solution must be maintained at 60oC constantly throughout the experiment. Last but not least,
the time of cleaning the short path distillation column should be prolonging to ensure that the
path was cleaned from the ethylene glycol residue.
6.0 REFERENCES
H.B Moller, S.G. Sommer, B.K. Ahring (2002). Separation Efficiency and Particle Size
Distribution in Relation to Manure Type and Storage Conditions
Hickman, K.C.D (2002-05-01). “High-Vacuum Short-path Distillation-A Review.” Chemical
Reviews 34(1): 51-106.doi: 10.1021/cr60107a002
Michael Albers, Alzenau-Horstein (2012). Application of Short-Path Distillation for
Processing Edible Oils and Fats
Perry, Robert H. and Green, Don W. (1984). Perry’s Chemical Engineers” Handbook (6th ed.)
McGraw-Hill ISBN 0-7-049479-7
Sales-cruz, m, & Gani, R. (2005). Short-Path Evaporation for Chemical Product Modelling,
Analysis and Design
7.0 APPENDICES
Ethylene glycol-water The vacuum pump The distillate was collected

mixture was heated pressure was held at the left side whereas the
o constant at 200 mbar. bottom product was
constant at 60 C and
pumped at 10 rpm. collected at right side.
Overview of short path Both temperature and stirring speed were

distillation process. manipulated throughout the experiment to
study the effect on separation efficiency.
UNIT OPERATION LAB
(BKF3731)
Title of Experiment : Sieve Tray Distillation
Date of Experiment : 6 March 2018
List of Students :
Name Student’s ID
Group No. :3
Section : 02
Marks :
Title of Experiment : Sieve Tray Distillation

TABLE OF CONTENT
No. Title Page
1.0 Abstract 1
2.0 Introduction 2
3.0 Methodology 3
6.0 References 11
7.0 Appendices 12
1.0 ABSTRACT
Sieve tray distillation was a process of separating various components of a liquid solution
by using the sieve trays in which the separation depended on the distribution of these
components between a vapour and a liquid phase. The objective of this experiment was to
determine the effect of feed composition on the height equivalent theoretical plates (HETP) at
total reflux in sieve tray distillation. The experiment was started with the preparation of
calibration curve for a set of mixtures containing ethanol and water versus refractive index (RI)
by manipulating the concentration of ethanol at 0%, 25%, 50%, 75% 90% and 100%. Then, a
mixture of ethanol and water at composition of 50:50 was poured into reboiler and the reflux
control and heater power regulator were set at 0 position and 2000 W respectively. The time
for the first bubble to come out from the tray was recorded. The temperature for all trays and
reboiler were recorded when the top column temperature sensor TT 112 reached steady state
and the time to reach steady state also recorded. Next, the reflux control was set to position 1
and the timer was started when the level in phase separator reached 100 mL. The timer was
stopped when the distillate reached 200 mL and the flowrate of the distillate was determined.
The distillate and bottom product were collected to determine its refractive index. The
experiment was then repeated with a mixture of ethanol and water at composition of 60:40 and
70:30. The experimental result showed when the percentage of ethanol in water increased, the
refractive index also increased, the volumetric flowrate of the distillate also increased due to
its high volatility and vapour pressure. Besides, the percentage of ethanol in distillate was
higher than that in bottom due to the lower boiling point of ethanol when compared to water.
Furthermore, it was concluded that the higher the feed composition of ethanol in water, the
higher the number of theoretical trays, and hence the shorter the HETP at total reflux in sieve
tray distillation. The experiment was suggested to cool down first before continuing the
experiment for the next heating level to improve the accuracy of the result and the distillation
column was suggested to flush with distilled water to avoid contamination in the experiment
that caused by the impurities.
2.0 INTRODUCTION
Distillation separate various components of a liquid solution depends on the distribution of
these components between a vapour and a liquid phase. All components are present in both
phases. The vapour phase is created from the liquid phase by vaporization at the boiling point
Distillation is concerned with solutions where all components are appreciably volatile.
In tray distillation, the liquid (L) flow to the stage below and the vapour (V) flow upward
to the stage above. The vapour and liquid leaving the tray in equilibrium. Concentration of
more volatile component is being increased in the vapour from each stage going upward and
decreased in the liquid from each stage going downward. The final vapour product coming
overhead is condensed in a condenser and a portion of the liquid product (distillate) is removed
which contain high concentration of A. The remaining liquid from the condenser is returned
(refluxed) as a liquid to the top tray. The liquid leaving the bottom tray enters a reboiler where
it is partially vaporized and the remaining liquid which lean in A or rich in B is withdrawn as
liquid product. The vapour forms the reboiler is sent back to the bottom tray.
Various type of trays can be used in distillation such as sieve tray, valve tray and bubble
cap tray. This experiment is using sieve tray distillation for separating ethanol-water mixture.
Sieve tray is a type of column internal with simple metal plates with holes in them. The hole
sizes range from 3 to 12 mm in diameter, with 5 mm a common size. The vapor area of the
holes varies between 5 to 15% of the tray area. In the sieve tray, vapor bubbles up through
simple holes in the tray through the flowing liquid. The liquid is held on the tray surface and
prevented from flowing down through holes by the kinetic energy of the gas or vapor. The
depth of liquid on the tray is maintained by an overflow, outlet weir. The overflow liquid flows
into the downspout to the next tray below. (Geankoplis, 2003)
3.0 METHODOLOGY
Equipment / Apparatus / Material: Sieve Tray Distillation Unit, Refractometer, 5 L of binary
mixture (ethanol-water) at different composition, Beakers
3.1 Preparation of Calibration Curve
A set of mixtures containing ethanol and water was prepared:
(a) 0 mL Ethanol + 10 mL Water Refractive index (RI) for each mixture
(b) 2.5 mL Ethanol + 7.5 mL Water were determined by using a
(c) 5.0 mL Ethanol + 5.0 mL Water refractometer. The values were recorder
(d) 7.5 mL Ethanol + 2.5 mL Water and a calibration curve was plotted.
(e) 9.0 mL Ethanol + 1.0 mL Water
(f) 10 mL Ethanol + 0 mL Water
3.2 Experimental Procedure
5 L (2.5 L ethanol + All the remaining liquid left in All valves were closed
2.5 L water) of the system was discarded properly except V15 and
mixture was prepared. before starting the experiment. V14 for cooling purposes.
The main power The charge port cap in the reboiler B1

The reflux control was opened and the ethanol-water feed
was set at 0 position. switch on the control
panel was turned on. mixture was poured into the reboiler.
(total reflux) The charge port cap was then closed.
Cartridge heaters W1 was The time for the The temperature for all trays and
switch on and the heater first bubble to reboiler were recorded when the top
power regulator was set to come out from the column temperature sensor TT 112
2000 W. The timer was started tray was recorded. reached steady state. The time to reach
once the heater was set. steady state also recorded.
Valve V8 and V2 were Valve V9 was opened and The reflux control was set to position
opened to collect the the distillate sample was 1. (Total distillate offtake) The timer
bottom product collected by using beaker. was started when the level in phase
sample by using Valve V9 was then closed separator reached 100 mL. The timer
beaker. Valve V2 and and the reflux control was set was stopped when the distillate
V8 were then closed. to position 0. (Total reflux) reached 200 mL and the flowrate of the
distillate was determined.
The refractive index The heater was turned off and The experiment was repeated by using
of the bottom and all the liquid from the system different composition of ethanol and
distillate samples was discarded for the next water:
were measured. feed composition.
(a) 3 L Ethanol + 2 L Water
(b) 3.5 L Ethanol + 1.5 L Water
Standard Concentration (mol %) Refractive Index (RI)
Set 1 Set 2 Average
1 0 1.3361 1.3357 1.3359
2 25 1.3454 1.3404 1.3429
3 50 1.3456 1.3490 1.3473
4 75 1.3496 1.3492 1.3494
5 90 1.3502 1.3520 1.3511
6 100 1.3538 1.3546 1.3612
Figure 4.1: Calibration Curve of Refractive Index versus Concentration of Ethanol in Water
Figure 4.1 showed the calibration curve of refractive index versus concentration of
ethanol in water, where the slope = 0.0002 and y-intercept = 1.3364. The equation that related
refractive index to the composition was:
Refractive Index = 0.0002(concentration(mol %)) + 1.3364
From the calibration curve above, it showed that the refractive index was directly
proportional to the concentration of ethanol. The higher the concentration of ethanol, the higher
the value of refractive index and vice versa. From the data, the refractive index of pure ethanol
and pure water were 1.3612 and 1.3359 respectively.
4.2 Data Collection for Distillate and Bottom Product
Table 4.2: Time and Reboiler Temperature for First Vapour Formed
Feed Composition Time for First Vapour Formed Reboiler Temperature for First
(Ethanol: Water) (min) Vapour Formed (oC)
50:50 10.12 85.5
60:40 9.55 84.4
70:30 8.34 83.9
Table 4.3: Distillate Flow Rate

Feed Composition Time Taken from 100 mL to Distillate Flow Rate (mL/s)
(Ethanol: Water) 200 mL (s)
50:50 125.42 0.7973
60:40 109.31 0.9148
70:30 90.25 1.1080
Table 4.4: HETP at Steady State Temperature for Different Feed Composition
Feed Time to Distillate Reboiler Distillate Bottom HETP
Composition Reach Temperature Temperature RI %mol RI %mol (mm)
(Ethanol: Steady State at Steady at Steady EtOH EtOH
Water) Temperature State State
(min) (oC) (oC)
50:50 9.45 77.4 86.5 1.3492 64.00 1.3452 44.00 353.77
60:40 10.46 77.2 84.6 1.3505 70.50 1.3440 38.00 243.51
70:30 12.22 77.0 83.5 1.3512 74.00 1.3425 30.50 168.16
According to Table 4.3, when the mole fraction of ethanol in water increased, the
distillate flow rate decreased. This was because the volatility of the mixture increased, and thus
shorter time needed for the ethanol to evaporate from the water. Hence, the time taken for the
ethanol to fill from 100 mL to 200 mL was decreased. When the volatility of the mixture
increased, its vapour pressure at given temperature increased too. This high vapour pressure
will ease the liquid particles to escape from the liquid surface to form vapour. When the ethanol
was vaporized, it condensed immediately after passing through the condenser. The normal
boiling point of the mixture will decrease and thus the temperature to form the first drop of
distillate was lower.
In addition, based on Table 4.4, when the mole fraction of ethanol in water was
increased, the percentage of ethanol in distillate stream was increased whereas for that in
bottom stream was decreased. However, the percentage of ethanol in distillate stream was
higher than that in bottom stream since ethanol has lower boiling point than water. Hence,
heating the feed stream will evaporate the ethanol and the distillate will be rich of ethanol.
4.3 Calculation of HETP
Table 4.5 below showed the equilibrium data for the ethanol-water system at 1 atm obtained
from Perry’s Handbook. It was used to plot the ethanol-water equilibrium graph at 1 atm to
determine the theoretical number of plates at total reflux.
Table 4.5: Ethanol-Water Equilibrium Data at 1 atm from Perry’s Handbook
Temperature Mole Fraction of Ethanol in Mole Fraction of Ethanol in
o
( C) Liquid Phase, 𝒙𝐄 Liquid Phase, 𝒚𝐄
100 0.0000 0.0000
95.5 0.0190 0.1700
89 0.0721 0.3891
86.7 0.0966 0.4375
85.3 0.1238 0.4704
84.1 0.1661 0.5089
82.7 0.2337 0.5445
82.3 0.2608 0.5580
81.5 0.3273 0.5826
80.7 0.3965 0.6122
79.8 0.5079 0.6564
79.7 0.5198 0.6599
79.3 0.5732 0.6841
78.74 0.6763 0.7385
78.41 0.7472 0.7815
78.15 0.8943 0.8943
78.30 1.0000 1.0000
ETHANOL-WATER EQUILIBRIUM GRAPH

1.2
MOLE FRACTION OF ETHANOL IN VAPOR
Ethanol-Water Equilibrium line at 1atm 45 degree line

1
0.8
PHASE, YE
0.6
0.4
0.2
0
0 0.2 0.4 0.6 0.8 1 1.2
MOLE FRACTION OF ETHANOL IN LIQUID PHASE, XE
Figure 4.2: Ethanol-Water Equilibrium Graph

MOLE FRACTION OF ETHANOL IN VAPOR PHASE, YE ETHANOL-WATER EQUILIBRIUM GRAPH
1.2
0.8
0.6
0.4
0.2
0
0 0.2 0.4 0.6 0.8 1 1.2
Figure 4.3: McCabe-Thiele Diagram for Distillation of Ethanol-Water When the Feed
Consists of 50% Ethanol:50% Water Mixture

1.2
MOLE FRACTION OF ETHANOL IN VAPOR PHASE, YE

1
0.8
0.6
0.4
0.2
0
0 0.2 0.4 0.6 0.8 1 1.2
MOLE FRACTION OF ETHANOL IN VAPOR PHASE, YE
1.2
1
0.8
0.6
0.4
0.2
0
0 0.2 0.4 0.6 0.8 1 1.2
The height of equivalent theoretical plate (HETP) was calculated by using the following
equation:
H= n(HETP) (Geankoplis, 2003)
Where, n = number of theoretical trays (number of stages + 1 reboiler)
H = height of distillation column
From Figure 4.3, the theoretical stages needed were about 1.12. Hence, the number of
theoretical trays = 1.12 + 1 reboiler = 2.12 theoretical trays
According to the calculation above, it can be concluded that when the percentage of ethanol in
water increased, the number of theoretical trays required also increased. As the percentage of
volatile ethanol in the feed increased, the column efficiency will also increase because it will
give a better performance of distillation. Since the column with high plate number were
considered to be more efficient, (Agilent, n.d), this translated to a higher percentage of ethanol
feed, higher column efficiency, and higher number of plate per meter.
For this experiment, the total effective column height is 750 mm.
Table 4.6: HETP at Different Feed Composition
Feed Composition Theoretical Number of Trays HETP (mm)
(Ethanol: Water)
50:50 2.12 353.77
60:40 3.08 243.51
70:30 4.46 168.16
Based on Table 4.6, it showed that when the composition of ethanol in water increased from
50% to 70%, the HETP value decreased from 353.77 mm to 168.16 mm. HETP values
indicated the length of each theoretical plate, the shorter the length of each theoretical plate,
the higher the number of plate contained when the effective column height was fixed.
In a nutshell, based on the calibration curve, the higher the percentage of ethanol in
water, the higher the refractive index. From the experimental result, it can be concluded that as
the percentage of ethanol in water increased, the higher the volatility for the mixture, the shorter
the time for ethanol to fill from 100 mL to 200 mL, and hence causing the volumetric flow rate
to increase. Besides, the higher the volatility of the mixture, the higher the vapour pressure it
exerted, and thus causing the liquid particles to become easier to be vaporized followed by the
rapid condensation through condenser. Consequently, the normal boiling point decreased and
hence the temperature to form the first drop of distillate was lower. Moreover, as the percentage
of ethanol at the feed stream increased, the percentage of ethanol at distillate increased whereas
for that at bottom decreased. The percentage of ethanol in distillate stream was higher than that
in bottom stream due to the lower boiling point of ethanol. Furthermore, it can be sum up that
as the percentage of ethanol in water increased from 50% to 70%, the number of theoretical
trays increased from 2.12 trays to 4.46 trays, and hence the higher the efficiency of the column.
As a result, the height of equivalent theoretical plates (HETP) values also decreased from
353.77 mm to 168.16 mm. As the length of each theoretical trays decreased, the number of
trays when the effective column height that fixed at 750 mm also increased. In short, the higher
the percentage of ethanol in water, the higher the column efficiency, the lower the HETP values
as it was inversely proportional to the column efficiency and the number of theoretical trays.
As for the recommendation, the system should be cooled down first before proceeding
the experiment for the next heating level to improve the accuracy of the result. Secondly, the
refractometer should be wiped every time after used before to prevent the deviation of the
refractive index reading. This was important as the refractometer reading will affect the value
of the mole fraction of ethanol calculated. Other than that, all the solution in the distillate and
bottom should be drained out and flushed with distilled water after operation to ensure that the
next experiment was not contaminated with the impurities.
6.0 REFERENCES
Perry, Robert H. and Green, Don W. (1984). Perry’s Chemical Engineers” Handbook (6th ed.)
McGraw-Hill ISBN 0-7-049479-7
Technologies, A. (n.d.). Theoretical Plates Counts
7.0 APPENDICES
The time for the ethanol The distillate was The bottom product
to fill from 100 mL to 200 collected at the top. was collected at the
mL was recorded. reboiler.
Overview of sieve tray The time for the first The ethanol-water
distillation process. vapour formed on the mixture was poured
sieve trays was recorded. into the reboiler.
UNIT OPERATION LAB
(BKF3731)
Title of Experiment : Solid Liquid Extraction
List of Students :
Name Student’s ID
Group No. :3
Section : 02
Marks :
Title of Experiment : Solid Liquid Extraction

TABLE OF CONTENT
No. Title Page
1.0 Abstract 1
2.0 Introduction 2
3.0 Methodology 3
6.0 References 9
7.0 Appendices 10
1.0 ABSTRACT
Solid liquid extraction or leaching was the separation of solutes from solid phase by
contacting the solid with liquid. The objective of this experiment was to study the salt
extraction from sea-shore sand using solid-liquid extractor unit. Standard salt solutions of salt
concentration from 5 g/L to 30 g/L were prepared and its respective conductivity were
determined to plot the calibration curve. Firstly, 2 kg of sea-shore sand (in fibre bag) were
weighed and put into the vessel cover. The water was then filled carefully until the vessel
equator level. Next, the equipment was started up. 15 minutes after solvent had begun to pass
through the product cooler, flowrate FI 1 was measured. The values of TI 1 and PI 4 were
recorded when it reached steady state. The sample reboiler contents and effluent were taken
every 2 minutes for the first 10 minutes, then every 5 minutes until 30 minutes at T = 45. The
conductivity for each sample taken was determined. Based on the calibration curve, it could be
concluded that the conductivity increased linearly with the salt concentration. According to the
experimental result, it could be summarized that the salt concentration in reboiler increased
along with time from 5.3683 g/L to 15.8245 g/L due to the boiling point of water was lower
than salt whereas the salt concentration in effluent decreased along with time from 30.7119 g/L
to 0.5609 g/L due to the salt was being extracted from the sea-shore sand which eventually
causing the salt concentration in the sea-shore sand to be decreased. The final extraction yield
for the solid liquid extraction in this experiment was 66.08%. The solvent in this experiment
was suggested to be provided with large exchange area and short diffusion path to achieve
faster and most complete solid extraction.
2.0 INTRODUCTION
Extraction was a method used for the separation of organic compound from a mixture
of compound. This technique selectively dissolved one or more compounds into an appropriate
solvent. The solution of these dissolved compounds was referred to as the extract
(vlab.amrita.edu,2011).
Solid liquid extraction (or leaching) was the separation of a solid solute from a mixture
of solids by dissolving it in a liquid phase. Basically, there were three components in leaching:
solid solute, insoluble solids and solvent. In most cases, the diffusion of intra-particle soluble
component controlled the extraction rate. Therefore, the process was often called as diffusion
extraction. Generally, the process can be considered in two steps which were contacting step
and separation step. First, contact of solid with liquid and selective dissolution of one or more
components of the solid phases. It was a mass transfer step that by transferring the soluble
constituent from the solid phases into liquid phases by diffusion and dissolution. Next,
separation and recovery of the resulting solution from the residual solid. This was a momentum
transfer step that could be carried out by settling or filtration (El. Monsy et al,2016).
Solid liquid extraction unit had been designed to demonstrate the extraction process
whereby components could be selectively extracted from solid mixtures by using a suitable
solvent. Solid liquid extraction unit was complete with spherical vessels heating bath condenser,
reflux divider, extraction vessel and necessary pipelines and valve (Sardar et al, nd).
Solid liquid extraction was widely used in food, for instance: extraction of sugar from
sugar cane or sugar beet, isolation of vegetable oils from different seeds, pharmaceutical
industries, and in hydrometallurgy which was the leaching of metal ions from ores.
3.0 METHODOLOGY
Standard salt solutions were prepared at 5 g/L, 10 g/L, 15 g/L, 20 g/L, 25

g/L, 30 g/L and their conductivities were obtained.
2 kg of sea-shore sand was weighed out and put into the fibre bag. The
extraction vessel cover was opened, and fibre bag was placed into the
extraction vessel. The top of the bag was ensured open for downward
solvent flow. The vessel cover was replaced. The vent and solvent food
lines were replaced.
The charge valve 4 was opened. The water was filled carefully until the
vessel equator level.
The solvent feed line from below the distillate cooler was ensured to be
firmly attached to the top of the extraction vessel. V5 was closed. The
equipment was started up.
15 minutes after solvent had begun to pass through the product cooler,
flowrate FI 1 was measured. The values of TI 1 and PI 4 were recorded.
A sample from the reboiler was taken carefully by open sampling valve
V2. Valve V2 was closed after sample was removed.
Valve V5 was closed and solvent transfer to the extraction vessel was
begun.
A sample of the first effluent was taken by opening sampling valve V3.
The collection of this sample was recorded at T = 0.
The sample reboiler contents and effluent were taken every 2 minutes for
the first 10 minutes, then every 5 minutes until 30 minutes at T = 45. The
conductivity for each sample taken was determined.
The final temperature indicated by TI 1 was recorded.
The equipment was shut down by following the instruction in part of

General Shut Off Procedures in Work Instruction.
The standard solution was prepared by dissolving salt in 200 mL distilled water.
Example: For 1 g of salt,
1g
Salt Conc = = 5 g/L
0.2 L
Salt Concentration Conductivity Reading 1 Conductivity Reading 2 Average
Standard
(g/L) (mS/cm) (mS/cm) (mS/cm)
1 5 12.0 19.2 15.6
2 10 23.6 25.8 24.7
3 15 36.7 36.5 36.6
4 20 45.9 46.1 46.0
5 25 52.3 53.1 52.7
6 30 64.6 63.2 63.9
Conductivity versus Salt Concentration

70
Conductivity (mS/cm)
60
50
40
30
y = 1.9137x + 6.4267
20 R² = 0.9955
10
0
0 5 10 15 20 25 30 35
Salt Concentration (g/L)
Figure 4.1: Calibration Curve of Conductivity versus Salt Concentration
Figure 4.1 showed the calibration curve of conductivity versus salt concentration, where
the slope = 1.9137 and y-intercept = 6.4267. The equation that related conductivity to the salt
concentration was:
𝐠
𝐂𝐨𝐧𝐝𝐮𝐜𝐭𝐢𝐯𝐢𝐭𝐲 = 𝟏. 𝟗𝟏𝟑𝟕 (𝐬𝐚𝐥𝐭 𝐜𝐨𝐧𝐜𝐞𝐧𝐭𝐫𝐚𝐭𝐢𝐨𝐧( )) + 𝟔. 𝟒𝟐𝟔𝟕
𝐋
From the calibration curve above, it showed that the conductivity was directly proportional to
the salt concentration. The higher the salt concentration, the higher the value of conductivity
value and vice versa. Conductivity was the ability of the electrolyte solution to conduct
electricity as the solution containing anions and cations. The conductivity increased due to the
presence of sodium ions, Na+ and hydroxide ions, OH- in the salt solution.
4.2 Experimental Result

Weight of solid charge: 2 kg TI 1 (Final) : 110oC
FI 1 : 1.40 mL/s PI. 4 : 2 bar
TI 1 (Initial) : 40oC
Table 4.2: Experimental Data of the Conductivity and Salt Concentration at
the Reboiler and Effluent
Reboiler Effluent
Salt Salt
Time Conductivity Conductivity
Concentration Concentration
(min) (mS/cm) (mS/cm)
(g/L) (g/L)
0 16.70 5.3683 65.2 30.7119
2 19.34 6.7478 60.47 28.2402
4 20.89 7.5578 45.80 20.5744
6 22.19 8.2371 36.61 15.7722
8 23.67 9.0105 29.43 12.0203
10 25.21 9.8152 23.12 8.7230
15 28.78 11.6807 18.12 6.1103
20 29.80 12.2137 11.8 2.8078
25 31.02 12.8512 9.33 1.5171
30 33.51 14.1523 8.25 0.9528
35 35.49 15.1870 7.91 0.7751
40 36.71 15.8245 7.50 0.5609

Table 4.2 above showed the conductivity at the reboiler and effluent at different time
intervals. The salt concentration at each time interval can be determined by using the equation
obtained from the calibration curve, y = 1.9137x + 6.4267 where y = conductivity and x = salt
concentration. The experiment was stopped after 40 minutes because the salt concentration
obtained did not differ much and the water in the tank was fully used.
The final extraction yield for the solid liquid extraction in this experiment was 66.08%
which can be calculated as shown below:
15.8245−5.3683
Final extraction yield (%) = x 100% = 66.08%
15.8245
Salt Concentration in Reboiler versus Time

18.00
Salt Concentration (g/L)
16.00
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
0 5 10 15 20 25 30 35 40 45
Time(min)
Figure 4.2: Graph of Salt Concentration in Reboiler versus Time
Figure 4.2 above showed the graph of salt concentration in reboiler against time. The
graph showed the salt concentration increased as the time of extraction increased. As the
conductivity increased along with the time, it can be concluded that the salt concentration was
increasing in the reboiler. As the boiling point of salt was higher than that of water, the salt
remained inside the reboiler instead of vaporizing with water, causing the accumulation of the
salt inside the reboiler (Geankoplis, 2003). The salt, had high boiling temperature of 1413oC.
The lower boiling point water, will first vaporized as the temperature achieved 100oC and as
the result the salt will accumulate inside the reboiler causing its concentration to be increased
over the time (Geankoplis, 2003). More and more salt was extracted from the sea-shore sand
by water from time to time and passed into the reboiler and only distilled water was evaporated
in the reboiler. Consequently, this had caused the concentration of the salt to increase
accordingly with the time. Eventually, the salt concentration increased gradually from 5.3683
g/L to 15.8245 g/L.
Salt Concentration in Effluent versus Time

35
30
Salt Concentration(g/L)
25
20
15
10
0
0 5 10 15 20 25 30 35 40 45
Time(min)
Figure 4.3: Graph of Salt Concentration in Effluent versus Time
According to Figure 4.3, it showed the salt concentration in effluent deceased along
with the time. The salt concentration decreased as the conductivity decreased along with the
time. This was because as the salt was being extracted from the sea-shore sand, the salt
concentration in the sea-shore will be decreased. Thus, the rate of dissolution of salt into solvent
decreased and the conductivity reading was decreased too along with the time. As a result, the
salt concentration in effluent decreased drastically from 30.7119 g/L to 0.5609 g/L. When the
effluent concentration decreased to zero, this indicated that the salt had been fully extracted.
In a nutshell, the calibration curve showed that the higher the salt concentration, the
higher the conductivity. From the experimental result, it can be concluded that the salt
concentration in reboiler increased along with time from 5.3683 g/L to 15.8245 g/L as the
conductivity showed increased trend. This phenomenon occurred because the boiling point of
water was lower than salt and thus the water was being vaporized while the salt was
accumulated in the reboiler. Meanwhile, the salt concentration in effluent decreased along with
time from 30.7119 g/L to 0.5609 g/L due to the salt was being extracted from the sea-shore
sand which eventually causing the salt concentration in the sea-shore sand to be decreased.
Hence, the conductivity showed a declining trend in the effluent. The final extraction yield for
the solid liquid extraction in this experiment was 66.08%.
For the recommendation, the pressure of the solid liquid extraction unit should not
exceed 2 bars so that it will not influence the result. Moreover, it was recommended that to use
different types of solvent and raw material to compare the performance of extraction unit such
as rose petals and diethyl ether can be used to extract the rose essential oil. Furthermore, the
solvent must be provided with large exchange surface and short diffusion path to achieve the
faster and most complete solid extraction.
6.0 REFERENCES
El. Monsy, Nagwa(2016). Solid-Liquid Extraction. Retrieved from Slide player:

http://slideplayer.com/slide/3953611
Sardar Estate, Vadodura. Gujerat.(n.d) Liquid Extraction Retrieved from
http://www.indiamart.com/mahavir-scientific/liquid-extraction-systems.
vlab.amrita.edu,. (2011). Extraction of Caffeine from Tea. Retrieved 16 March 2018, from
vlab.amrita.edu/?sub=3&brch=64&sim=169&cnt=1
7.0 APPENDICES
2 kg of sea-shore sand 40 mL of sample was 40 mL of sample was

was weighed and collected from effluent collected from reboiler
placed into a fibre bag. stream. stream.
Overview of solid The flowrate FI 1 was The values of TI 1 and

liquid extraction unit. measured. PI 4 were recorded.
UNIT OPERATION LAB
(BKF3731)
Title of Experiment : Absorption Column Unit
List of Students :
Name Student’s ID
Group No. :3
Section : 02
Marks :
Title of Experiment : Absorption Column Unit

TABLE OF CONTENT
No. Title Page
1.0 Abstract 1
2.0 Introduction 2
3.0 Methodology 3
6.0 References 9
7.0 Appendices 10
1.0 ABSTRACT
Absorption column was one of the separation techniques that involved liquid and gas.
One or more component of a gas mixture can be separated when a certain liquid flow through
it counter-currently. The objective of this experiment was to determine the effect of air flow
rate and water flow rate on flooding point and pressure drop in an absorption column. There
were two parts in this experiment. First, part one was to determine the pressure drop and
flooding point at different water flow rate. The water flow rate was set at 2.5 L/min with air
flow rate at 100 L/min. After 3 minutes, the air flow rate was increased by 10 L/min interval
until the flooding point was observed. The part one experiment was repeated for water flow at
3.0 L/min and 3.5 L/min respectively. Next, the second part of this experiment was to determine
the pressure drop and flooding point at different air flow rate. The air flow rate was set at 100
L/min with air flow rate at 2.0 L/min. After 3 minutes, the water flow rate was increased by
0.5 L/min interval until the flooding point was observed. The part two experiment was repeated
for water flow rate at 110 L/min and 120 L/min respectively. Based on the result of this
experiment, when the water flow rate increased from 2.5 L/min to 3.5 L/min, the time took to
reach flooding point was decreased from 15 minutes to 6 minutes. This phenomenon was due
to the increased amount of water flowing down in the absorption column per unit time which
eventually caused the water to be holdup in the packing. In the meantime, when the air flow
rate increased from 100 L/min to 120 L/min, the time taken to reach flooding point decreased
from 15 minutes to 9 minutes due to the increased amount of air flowing up in the absorption
column which eventually entrained the water movement and caused the accumulation of water
in the packings. Moreover, when the water flow rate increased from 2.5 L/min to 3.5 L/min at
constant air flow rate of 110 L/min, the pressure drop in the column increased from 9.59 cm
H2O to 51.80 cm H2O packings due to the increased in the fluid friction between water flow
and the packings which eventually caused the down flowing water to encounter large resistance.
Similarly, when the air flow rate increased from 100 L/min to 120 L/min at constant water flow
rate of 2 L/min, the pressure drop increased too from 8.82 cm H2O to 13.90 cm H2O due to the
greater resistance encountered by the up flowing air that resulted from the fluid friction
between air flow and the packings. Lastly, the experiment was recommended to be carried out
by using different sizes of packing to compare the performance of the absorption unit.
2.0 INTRODUCTION
Gas absorption was a process in which the soluble part of a gas mixture is transferred
to or dissolved in a liquid. The reverse process, called desorption or stripping, was used to
transfer volatile parts from a liquid mixture to gas. Therefore, there will be mass transfer of the
component of the gas from the gas phase to the liquid phase. The solute transferred was said to
be absorbed by the liquid. In gas desorption (or stripping), the mass transfer was in the opposite
direction, of which the transfer was from the liquid phase to the gas phase. The principles for
both systems were the same. But from here and on, we were only interested gas absorption.
There were two types of absorption process; physical absorption and chemical
absorption, depending on whether there was any chemical reaction between the solute and
solvent (absorbent). In addition, flooding point was a phenomena where the liquid began to
spray out from the column (T.Takahashi, 1967). At this point, the pressure drop rose
dramatically. The gas velocity that corresponding to the flooding point was called flooding
velocity. Beyond this velocity, the liquid was unable to flow down the column (Hewitt, 1963).
The saddle packed material in the absorption column was used to increase the contact
surface area which enhanced the efficiency and shortened the duration of the process. The
advantages of using packed absorption column was low liquid holdup, cheaper construction,
and suitable for vacuum service and foaming service (Chattopadhyay, 2007).
3.0 METHODOLOGY
Equipment / Apparatus / Material: Packed Absorption Column, Air Compressor, Water and
Air, Stopwatch
1. The valves for right column for saddle pack were opened.
2. The water flow rate was set at 2.5 L/min.
3. The air flow rate was set at 110 L/min. The stop watch was started and left for
3 minutes. The water and air flow rate were kept constant from time to time.
4. After 3 minutes, the data for pressure drop, ΔP was taken from Digital ΔP
Meter.
5. Step 3 and 4 were repeated by increasing the air flow rate by 10 L/min
interval until the flooding point was observed.
6. Step 3 to 5 were repeated for water flow rate at 3.0 L/min and 3.5 L/min.
7. Next, the second experiment was run at different air flow rate of 100 L/min,
110 L/min, and 120 L/min at the increasing water flow rate by 0.5 L/min
interval until the flooding point was observed.
8. Step 4 was repeated.
9. The equipment was shut down according to the instructions in General Shut
Down Procedure.
Part A: Pressure Drop and Flooding Point at Different Water Flow Rate
Water flow rate, W Air flow rate, G Pressure drop, ∆P Time to reach
(L/min) (L/min) (cm H2O) flooding point
(every 3 minutes)
2.5 110 9.59 3
120 13.80 6
130 23.00 9
140 43.80 12
150 50.30 15
3.0 90 9.43 3
100 21.10 6
110 38.40 9
120 58.50 12
130 61.00 15
3.5 70 6.20 3
80 11.40 6
90 12.60 9
100 49.90 12
110 51.80 15
*Yellow colour indicated flooding point
Part B: Pressure Drop and Flooding Point at Different Air Flow Rate
Air flow rate, G Water flow rate, W Pressure drop, ∆P Time to reach
(L/min) (L/min) (cm H2O) flooding point
(every 3 minutes)
100 2.0 8.82 3
2.5 9.67 6
3.0 13.50 9
3.5 39.00 12
4.0 56.40 15
110 2.0 11.06 3
2.5 13.50 6
3.0 27.60 9
3.5 48.80 12
4.0 60.90 15
120 1.0 7.08 3
1.5 9.34 6
2.0 13.90 9
2.5 18.27 12
3.0 31.50 15
*Yellow colour indicated flooding point
Time versus Water Flow Rate
20
15
Time (min)
10
0
0 0.5 1 1.5 2 2.5 3 3.5 4
Water Flow Rate, W (L/min)
Figure 4.1: Graph of Time to Reach Flooding Point Versus Water Flow Rate
According to Figure 4.1, the time took to reach flooding point was decreasing with the
increasing water flow rate. At water flow rate of 2.5 L/min, it took 15 minutes to reach the
flooding point with air flow rate of 150 L/min. When water flow rate was increasing to 3.0
L/min, the time took to achieve flooding point was 12 minutes with the air flow rate of 120
L/min. Lastly, at water flow rate of 3.5 L/min, it took 6 minutes to reach the flooding point
with air flow rate of 80 L/min. The reason why this phenomenon occurred was because the
increasing water flow rate caused the amount of water flowing into the absorption column per
unit time to be increased. Consequently, large amount of water holdup in the packing and
resulted in shorter time required to achieve flooding point.
Time versus Air Flow Rate

16
14
12
Time (min)
10
8
6
4
2
0
95 100 105 110 115 120 125
Air Flow Rate, G (L/min)
Figure 4.2: Graph of Time to Reach Flooding Point Versus Air Flow Rate
Based on Figure 4.2, the graph showed that the time took to reach flooding point was
decreasing linearly with the increasing air flow rate. At air flow rate of 100 L/min, it took 15
minutes to reach the flooding point with water flow rate of 4 L/min. When air flow rate was
increasing to 110 L/min, the time took to achieve flooding point was 12 minutes with the water
flow rate of 4.5 L/min. Lastly, at air flow rate of 120 L/min, it took 9 minutes to reach the
flooding point with water flow rate of 2.0 L/min. The result showed that when the air flow rate
was increased, this caused the amount of air flowing into the absorption column per unit time
to be increased. As a result, the water movement entrained by the excessive air flow as the free
area of the air flow was decreasing. Eventually, the water holdup and accumulated in the
packing and hence the flooding point achieved at a shorter time.
Pressure Drop versus Water Flow Rate

60
Pressure Drop, ∆P (cm H 2O)
50
40
30
20
10
0
0 0.5 1 1.5 2 2.5 3 3.5 4
Water Flow Rate, W (L/min)
Figure 4.3: Graph of Pressure Drop Versus Water Flow Rate at Constant Air Flow Rate
(110 L/min)
From Figure 4.3, the pressure drop was increased proportionally to the water flow rate.
At constant air flow rate of 110 L/min, the pressure drop in the absorption column of 9.59 cm
H2O was recorded when the water flow rate was at 2.5 L/min. Next, when the water flow rate
increased to 3 L/min and 3.5 L/min, the pressure drop of 38.40 cm H2O and 51.80 cm H2O
were recorded respectively in the absorption column. J.Stichlmair (1998) stated that the
pressure drop was the result of fluid friction between water flow and the packings. Thus, when
the water flow rate increased at constant air flow rate, the fluid friction in the column will be
increased as well and hence the greater resistance encountered by the down-flowing water will
eventually result in the increased of pressure drop across the packings.
Pressure Drop versus Air Flow Rate
16
14
Pressure Drop, ∆P (cm H 2O)
12
10
8
6
4
2
0
95 100 105 110 115 120 125
Air Flow Rate, G (L/min)
Figure 4.4: Graph of Pressure Drop Versus Air Flow Rate at Constant Water Flow Rate
(2 L/min)
Figure 4.4 illustrated the relationship between pressure drop with the air flow rate. The
graph showed the pressure drop in the absorption column was increasing linearly with the
increasing air flow rate. At constant water flow rate of 2 L/min, the pressure drop in the
absorption column of 8.82 cm H2O was recorded when the air flow rate was at 100 L/min. Next,
when the air flow rate increased to 110 L/min and 120 L/min, the pressure drop of 11.06 cm
H2O and 13.90 cm H2O were recorded respectively in the absorption column. Pressure drop
was the result of fluid friction between air flow and the packing. Thus, when the air flow rate
increased at constant water flow rate, the fluid friction in the column will be increased as well
and hence the greater resistance encountered by the up flowing air will eventually result in the
increased of pressure drop across the packings.
In a nutshell, the higher the water flow rate, the shorter the time took to achieve flooding
point due to the increased amount of water flowing down in the absorption column per unit
time which eventually caused the water to be holdup in the packing. Besides, it was concluded
that the higher the air flow rate, the shorter the time took to achieve flooding point due to
increased amount of air flowing up in the absorption column which eventually entrained the
water movement and caused the accumulation of water in the packings. Moreover, when the
water flow rate increased at constant air flow rate, the pressure drop was found to be increased
in the packings due to the increased in the fluid friction between water flow and the packings
which eventually caused the down flowing water to encounter large resistance. Similarly, the
pressure drop also increased when the air flow rate was increasing at constant water flow rate
due to the greater resistance encountered by the up flowing air that resulted from the fluid
friction between air flow and the packings.
For the recommendation, the experiment can be carried out by using different sizes of
packing to compare the performance of the absorption unit. Moreover, it was suggested to study
the effect of pressure drop and flooding time in the absorption column unit by using Flexi rings
random packing. Furthermore, structured packing was also recommended for the experiment
as it can be carried out with very low pressure drop.
6.0 REFERENCES
Chattopadhyay, P. (2007). Absorption & stripping. New Delhi: Asian Books Private Limited.
Hewitt, G. (1963). Flooding and Associated Phenomena in Falling Film Flow in a Tube.
Scitech.
J. Stichlmair, J.B. (1998). General model for prediction of pressure drop and capacity of
counter current gas/liquid packed columns. 1-10.
T.Takahshi, K.F. (1967). A correlation of flooding velocities in counter current Gas-Liquid

Contactor of Column Type. Memoirs of the School of Engineering, Okayama University, Vol.
2, No. 1, 1-7.
7.0 Appendices
Overview of absorption column unit. The process flow diagram of the

absorption column unit.
The air flow rate can be adjusted. The pressure drop will be shown at
digital pressure drop meter.
UNIT OPERATION LAB
(BKF3731)
Title of Experiment : Tray Drying
List of Students :
Name Student’s ID
Group No. :3
Section : 02
Marks :
Title of Experiment : Tray Drying

TABLE OF CONTENT
No. Title Page
1.0 Abstract 1
2.0 Introduction 2
3.0 Methodology 3
6.0 References 12
7.0 Appendices 13
1.0 ABSTRACT
Drying was a process of removal of relatively small amounts of water from material.
One of the example of drying equipment was tray dryer. The objective of this experiment was
to study the effect of heating levels on drying rate. At first, 50 g of macaroni was soaked in
boiled water for about 10 minutes and then tossed. The balance was tared without the drying
tray. Next, the drying tray was put in the dryer and the weight was recorded. The 50 g boiled
macaroni was spread on the tray and the new weight and exposed area of the macaroni on the
tray were measured. After that, the fan level and heating level were set to the level 2 and then
switched on. The stopwatch was started to count the drying time. The inlet and outlet humidity
and temperature were recorded for every 5 minutes. The anemometer was used to measure the
air velocity and air flow rate. The experiment was repeated with heating rate level 4 and 6.
Based on the plotted graph of weight of wet macaroni versus time, it showed that the weight
of the wet macaroni decreased along with the time. At heating rate level 6, the graph showed
the steepest gradient as the loss of the moisture content occurred at higher rate due to the higher
heat energy supplied which resulted in the higher inlet air temperature. Likewise, the graph of
the free moisture content of the wet macaroni versus time also illustrated a declining trend. At
heating level 6, the free moisture content of the macaroni decreased faster than that at heating
level 2 and 4 due to the rapid declining of the moisture content and equilibrium moisture
content of the wet macaroni. Moreover, the graph of drying rate versus free moisture content
showed a similar trend which involved constant and falling rate period. From the graph, it can
be summarised that the drying rate of the wet macaroni at heating rate level 6 was the highest
among the others. For instance, critical moisture content of the wet macaroni can be determined
from the graph. The wet macaroni in this experiment was suggested to be spread and distributed
evenly on the tray as one layer to maximise the exposed area for the drying process.
2.0 INTRODUCTION
Drying is an essential unit operation in the chemical process industries with applications
ranging from forest products, and mineral processing to food products and pharmaceuticals.
Drying can be defined as the vaporization and removal of water or other liquids from a solution,
suspension, or other solid-liquid mixture to form a dry solid (“Solids Drying: Basics and
Applications,” 2017). One of the example of drying equipment was tray dryer.
Tray dryer, also called as shelf, cabinet, or compartment dryers was normally used to
dry, lumpy or pasty solid material. The material was spread uniformly on a removable metal
trays to a depth of 10 to 100 mm (Geankoplis, 2003). When the heat was added to the drying
air, the rate of drying increased, depending on the selected drying temperature and air velocity
(Jayas and Sohkansanj, 1989).
In tray dryer, drying was imposed by the heated air, which was recirculated by fan over
and parallel to the surface of the trays. During this process, about 10 to 20% of the fresh air
was passing over the trays, whereas the reminding was the recirculated air to remove bound
water or moisture content (Geankoplis, 2003).
The moisture that can be removed by drying under the given percent relative humidity
was called free moisture. The free moisture content, X can be calculated as follows (Geankoplis,
2003):
𝑊−𝑊𝑠
Moisture content, Xt = 𝑊𝑠
Free moisture content, X = Xt – X*
where W = weight of wet solid at given time, Ws = weight of dry solid, Xt = moisture content
of solid substance, X* = equilibrium moisture content of solid substance.
The rate of drying, R was
𝐿𝑠 𝑑𝑋
R=- 𝐴 𝑑𝑡
where, Ls = weight of dry macaroni used; A = exposed surface area for drying; dX/dt = slopes
of tangents at different values of t.
Application of tray dryer was widely used in agricultural drying because of its simple
design and capability to dry products at high volume. However, the greatest drawback of
the tray dryer was uneven drying because of poor airflow distribution in the drying chamber
(Misha et al., 2013).
3.0 METHODOLOGY
Material : Macaroni
Apparatus : Tray, Weighing balance, Anemometer, Stopwatch, Spatula
50 g of macaroni was soaked in boiled water for about 10 minutes and then tossed.
The balance was tared without the drying tray. The drying tray was put in the
dryer and the weight was recorded.
The 50 g boiled macaroni was spread on the tray. The new weight and exposed
area of the macaroni on the tray were measured.
The fan level and heating level were set to the level 2. The fan and heater were
then switched on. The stopwatch was started to count the drying time.
The inlet and outlet humidity and temperature were recorded for every 5 minutes.
The anemometer was used to measure the air velocity and air flow rate.
The experiment was repeated with heating rate level 4 and 6.

Heating Rate Level :2
Air Velocity : 1.92 m/s
Air Flowrate : 1193 x 10 cmm
Weight of tray + macaroni (g) : 350 g + 84.65 g = 434.65 g
Weight of dried macaroni (g) : 50 g
Macaroni surface area for drying : 13 cm x 16.5 cm = 214.50 cm2
Table 4.1: Data Collection for Heating Rate Level 2

Time Weight of Weight of Air Air Percentage Percentage Moisture Equilibrium Free
(min) Tray + Wet Temperature Temperature Relative Relative Content, Xt Moisture Moisture
Macaroni Macaroni Inlet, T1 (oC) Outlet, T2 Humidity Humidity (kg H2O/kg Content, X* Content, X
(g) (g) (oC) Inlet, H1 Outlet, H2 dry solid) (kg H2O/kg (kg H2O/kg
(% rF) (% rF) dry solid) dry solid)
0 434.65 84.65 30.3 30.2 30.3 67.2 0.6930 0.1600 0.5330

5 433.22 83.22 30.4 30.2 29.1 65.7 0.6644 0.1550 0.5094
10 432.13 82.13 30.4 30.4 28.8 65.4 0.6426 0.1525 0.4901
15 431.02 81.02 30.5 30.5 28.1 63.8 0.6204 0.1475 0.4729
20 430.21 80.21 30.7 30.5 27.6 62.6 0.6042 0.1463 0.4579
25 429.41 79.41 30.8 30.6 27.2 62.5 0.5882 0.1463 0.4419
30 429.03 79.03 30.8 30.6 27.2 62.4 0.5806 0.1450 0.4356
35 428.82 78.82 30.8 30.6 27.1 62.3 0.5763 0.1450 0.4313
40 428.71 78.71 30.8 30.7 26.9 62.0 0.5742 0.1450 0.4292

Time Weight of Weight of Air Air Percentage Percentage Moisture Equilibrium Free
0 432.96 82.96 30.9 30.8 26.8 61.7 0.6592 0.1438 0.5154

5 430.97 80.97 30.9 30.8 26.7 61.5 0.6193 0.1425 0.4768
10 429.36 79.36 31.1 30.9 26.5 61.3 0.5871 0.1425 0.4446
15 427.96 77.96 31.1 31.0 26.3 61.2 0.5592 0.1425 0.4167
20 426.60 76.60 31.1 31.0 26.1 60.5 0.5320 0.1418 0.3902
25 425.17 75.17 31.1 31.0 25.9 59.6 0.5033 0.1388 0.3645
30 423.92 73.92 31.2 31.1 25.8 59.1 0.4784 0.1375 0.3409
35 423.27 73.27 31.2 31.1 25.3 58.9 0.4654 0.1363 0.3291
40 422.95 72.95 31.2 31.1 24.9 58.6 0.4590 0.1363 0.3227

Time, t Weight of Weight of Air Air Percentage Percentage Moisture Equilibrium Free
0 426.78 76.78 40.0 39.7 0.4 6.2 0.5356 0.0375 0.4981

5 423.76 73.76 41.3 40.8 0.4 5.8 0.4752 0.0350 0.4402
10 421.47 71.47 42.1 41.4 0.4 5.3 0.4294 0.0338 0.3956
15 419.58 69.58 42.5 41.6 0.3 5.1 0.3916 0.0325 0.3591
20 417.81 67.81 43.0 42.5 0.3 4.8 0.3561 0.0313 0.3248
25 416.08 66.08 43.4 42.9 0.3 4.4 0.3215 0.0300 0.2915
30 414.47 64.47 44.1 43.3 0.3 4.4 0.2893 0.0300 0.2593
35 413.36 63.36 44.9 44.0 0.2 4.1 0.2671 0.0288 0.2383
40 412.92 62.92 45.2 44.6 0.2 4.1 0.2584 0.0288 0.2296
Table 4.4: Calculation of Drying Rate for Heating Rate Level 2, 4 and 6
Time, Heating Rate Level 2 Heating Rate Level 4 Heating Rate Level 6
t Free ∆𝑿 (kg ∆𝒕 Drying Free ∆𝑿 (kg ∆𝒕 Drying Free ∆𝑿 (kg ∆𝒕 Drying
(min) Moisture H2O/kg (min) Rate, R Moisture H2O/kg (min) Rate, R Moisture H2O/kg (min) Rate, R
Content, dry (g/min.cm2) Content, dry (g/min.cm2) Content, dry (g/min.cm2)
X (kg solid) X (kg solid) X (kg solid)
H2O/kg H2O/kg H2O/kg
dry dry dry
solid) solid) solid)
0 0.5330 0.0236 5 0.0011 0.5154 0.0386 5 0.0018 0.4981 0.0579 5 0.0027

5 0.5094 0.0193 5 0.0009 0.4768 0.0322 5 0.0015 0.4402 0.0446 5 0.0021
10 0.4901 0.0172 5 0.0008 0.4446 0.0279 5 0.0013 0.3956 0.0365 5 0.0017
15 0.4729 0.0150 5 0.0007 0.4167 0.0265 5 0.0012 0.3591 0.0343 5 0.0016
20 0.4579 0.0160 5 0.0007 0.3902 0.0257 5 0.0012 0.3248 0.0333 5 0.0016
25 0.4419 0.0063 5 0.0003 0.3645 0.0236 5 0.0011 0.2915 0.0322 5 0.0015
30 0.4356 0.0043 5 0.0002 0.3409 0.0118 5 0.0006 0.2593 0.0210 5 0.0010
35 0.4313 0.0021 5 0.0001 0.3291 0.0064 5 0.0003 0.2383 0.0087 5 0.0004
40 0.4292 - - - 0.3227 - - - 0.2296 - - -
Weight of Wet Macaroni versus Time
90
85
Weight of Wet Macaroni (g)
80
75
70
65
60
0 5 10 15 20 25 30 35 40 45
Time (min)
Heating Rate Level 2 Heating Rate Level 4 Heating Rate Level 6
Figure 4.1: Graph of Weight of Wet Macaroni Versus Time
Based on Figure 4.1, the graph showed that the weight of wet macaroni was decreasing
exponentially along with the time at heating rate level 2, 4 and 6. The line graph for heating
rate level 6 was the steepest among all the heating rate levels which indicated the weight of wet
macaroni was decreasing rapidly along with the time. This phenomenon occurred because
heating rate level 6 supplied more heat energy than the heating rate level 2 and 4 which resulted
in the higher inlet air temperature. As a result, higher heat transfer rate at heating rate level 6
causing the water molecules in the macaroni to escape rapidly to the air which eventually lead
to the rapid decreasing of the weight of wet macaroni along with the time.
Free Moisture Content versus Time
0.55
0.5
Free Moisture Content, X
0.45
0.4
0.35
0.3
0.25
0.2
0 5 10 15 20 25 30 35 40 45
Time (min)
Figure 4.2: Graph of Free Moisture Content Versus Time
According to Figure 4.2, the graph of free moisture content versus time at heating rate
level 2, 4 and 6 showed a declining trend. The free moisture content of the wet macaroni at
heating rate level 6 decreased rapidly, followed by heating rate level 4 and 2. This was because
the free moisture content was affected by two parameters which were moisture content, Xt and
equilibrium moisture content, X* as showed in the equation below:
Free moisture content, X = Xt – X*
The moisture content, Xt can be calculated by using the following formula:
𝑊−𝑊𝑠
Moisture content, Xt =
𝑊𝑠
where, W = weight of wet macaroni at given time; Ws = weight of dry macaroni
Based on the result, the moisture content, Xt of the wet macaroni at heating rate level 6
decreased quickly with the time when compared to that at heating level 2 and 4. For instance,
the percentage relative humidity at the outlet also decreasing rapidly at heating rate level 6 due
to high heat energy supplied which resulted in the lower value of equilibrium moisture content,
X*. Consequently, this caused the free moisture content in wet macaroni at heating rate level 6
to fall steeply along with the time when compared to that at heating rate level 2 and 4.
Drying Rate versus Free Moisture Content
0.003
0.0025
0.002
Drying Rate, R
0.0015
0.001
0.0005
0
0.2 0.25 0.3 0.35 0.4 0.45 0.5 0.55
Free Moisture Content, X
Figure 4.3: Graph of Drying Rate Versus Free Moisture Content
Figure 4.3 illustrated the relationship between drying rate and free moisture content at
heating rate level 2, 4 and 6. All the graphs showed the similar trend with constant and falling
rate period. The critical free moisture content can be determined from the above graph which
located at the end of the constant rate period. The critical free moisture content, Xc at heating
rate level 2, 4 and 6 were 0.4579, 0.3645 and 0.2915 respectively. The obvious difference
between these three graphs was that the drying rate for the wet macaroni at heating rate level 6
was the highest among all the heating rate levels. This was because heating rate level 6 supplied
high heat energy to the wet macaroni which allowed the water molecules to be escaped to the
air rapidly and thus resulted in the high drying rate among others. The rate of drying, R can be
calculated by using following formula:
𝐿𝑠 𝑑𝑋
R=-
𝐴 𝑑𝑡
where, Ls = weight of dry macaroni used; A = exposed surface area for drying; dX/dt = slopes
of tangents at different values of t.
5.0 CONCLUSION AND RECOMMEDATION
In a nutshell, the weight of the wet macaroni decreased along with the time and it
decreased rapidly at heating rate level 6, followed by heating rate level 4 and 2 due to higher
heat energy was supplied at heating rate level 6 which resulted in the higher inlet air
temperature. Moreover, it can be concluded that the free moisture content of the wet macaroni
at heating rate level 6 decreased steeply with the time when compared to that at heating rate
level 2 and 6 due to the rapid declining of the moisture content and equilibrium moisture
content of the wet macaroni. Furthermore, the graph of drying rate versus free moisture content
showed a similar trend which involved constant and falling rate period. From the graph, it can
be summarised that the drying rate of the wet macaroni at heating rate level 6 was the highest
among the others. For instance, critical moisture content of the wet macaroni can be determined
from the graph.
For the recommendation, the wet macaroni should be spread and distributed evenly on
the tray as one layer to maximise the exposed area for the drying process. Besides, the boiled
macaroni should be cooled down to room temperature before it is being put on the tray to make
sure that the drying rate will not affected by the temperature of the wet macaroni. Lastly, make
sure that there is no excess dripping water on the macaroni before it is being put on the tray for
drying.
6.0 REFERENCES
Jayas and Sokhansanj (1989). Thin layer drying of barley at low temperature, Canadian
Agricultural Engineering.
Misha, Suhaimi & Sohif, Mat & Ruslan, M.H. & Sopian, Kamaruzzaman & Salleh, Elias.
(2013). Review on the Application of a Tray Dryer System for Agricultural Products, World
Applied Sciences Journal.
Solids Drying: Basics and Applications - Chemical Engineering. (2017, November 20).
Retrieved from http://www.chemengonline.com/solids-drying-basics-and-
applications/?printmode=1
7.0 APPENDICES
Overview process of tray drying. The exposed surface area of the

macaroni on the tray was measured.
The weight of the macaroni Drying process of the wet

at given time was measured. macaroni in the tray dryer.
The inlet and outlet humidity The air velocity and air flowrate
and temperature at given time of the tray dryer were measured
were recorded. by using anemometer.

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UNIT OPERATION LAB

Title of Experiment : Crystallization

Date of Experiment : 10 April 2018

Instructor’s Name : Dr. Sumaiya Bt Zainal Abidin @ Murad

1. Arics Chieng Kie Siong KA15073

2. Rhakesh a/l Gandhi KA15133

3. Lim Hui Lun KA15184

4. Divya Nandhini KA17343

FACULTY OF CHEMICAL AND NATURAL RESOURCES ENGINEERING

UNIVERSITI MALAYSIA PAHANG

Please keep for student reference.

Submitted by; Received by;

(ARICS CHIENG KIE SIONG) ( )

Subject Code : BKF3731 Date Submitted: 17 April 2018

Title of Experiment : Crystallization

4.0 Results and Discussions 6

5.0 Conclusion and Recommendation 13

The general advantages of crystallization as a process were high purification can be

Step 3 and 4 were repeated with ethanol and water solvent.

The saturated solution was filtered to remove the excess salt.

3.3 Crash Cooling vs Natural Cooling Crystallization

Acetone T1 = 30 oC 35.4689 36.0310 35.7889 0.032 21346.195 35.3927

Solubility of Epsom Salt in Different Type of Solvents versus

Acetone Ethanol Water

∆Go = -RT ln Keq

∆Go = ∆Ho – T ∆So

The Keq was calculated using the following formula:

𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑆𝑎𝑙𝑡 (𝑔)

1/T versus ln Keq

Acetone Ethanol Water Linear (Acetone) Linear (Ethanol) Linear (Water)

Figure 4.2: Graph of 1/T Versus ln Keq for Different Solvents

4.2 Different Type of Crystal

Sugar 31.5165 35.2946 32.4934 0.0977

4.3 Crash Cooling Versus Natural Cooling Recrystallization

Dilution Theory and Problems. (n.d.). Retrieved from

Hallas N.J. (2011, February 2). Crystallization. doi:10.1615/AtoZ.c.crystallization

Recrystallization and Melting Points. (n.d.). Retrieved from

Zurich. (2008). Process Engineering Laboratory II Crystalizlation. Spring.

Nine crucibles were placed in the

The shapes of crystal

Title of Experiment : Thin Film Evaporation

Date of Experiment : 17 April 2018

Instructor’s Name : Dr. Sumaiya Bt Zainal Abidin @ Murad

1. Arics Chieng Kie Siong KA15073

2. Rhakesh a/l Gandhi KA15133

3. Lim Hui Lun KA15184

4. Divya Nandhini KA17343

FACULTY OF CHEMICAL AND NATURAL RESOURCES ENGINEERING

UNIVERSITI MALAYSIA PAHANG

Please keep for student reference.

Submitted by; Received by;

(ARICS CHIENG KIE SIONG) ( )

Subject Code : BKF3731 Date Submitted: 24 April 2018

Title of Experiment : Thin Film Evaporation

4.0 Results and Discussions 4

5.0 Conclusion and Recommendation 9

3.1 Preparation of Calibration Curve

3.2 Experimental Procedure

5 L of ethanol-water mixture at a composition of 60:40 v/v was prepared.

Equipment parts and function of the evaporator unit were identified.

The equipment was running for 7 minutes.

The distillate and bottom product flow rates were measured.

Refractive Index vs Concentration