Faculty of Chemical & Natural Resources Engineering

BKF3731
Unit operation lab

Sem. I - Session 2014/2015

Exp 1: Crystallizer
Exp 2: Thin Film Evaporator
Exp 3: Short Path Distillation
Exp 4: Sieve Tray Distillation
Exp 5: Solid Liquid Extractor Unit
Exp 6: Absorption Column Unit
Exp 7: Pressure Swing Adsorption

Instructor: Dr. Fatmawati Adam (coordinator), Ms. Nur Aminatulmimi Ismail, Dr.
Vo Nguyen Dai Viet

Teaching Engineer: Joharizal Johari , Hairul Hisham Ismail, Mohd. Hafiz Abd.
Latib, Mohd. Anuar Hj. Ramli, Zainal Giman, Zulhabri Khadisah

Fatmawati Adam/ Jolius Gimbun

 EXPERIMENT 1: CRYSTALLISER

Objective
1. To determine the solubility of Epsom salt (MgSO4) in ethanol, acetone and
toluene through vant Hoff Equation
2. To recrystallize MgSO4 using crash cooling crystallization.
3. To study crystal the shape of Epsom salt (MgSO4) in ethanol, acetone and
toluene.

Material
1. 200g Epsom salt (MgSO4)
2. 1L ethanol
3. 10ml ethanol
4. 10ml acetone
5. 10ml toluene

Apparatus:
1. 50ml beaker
2. Erlenmeyer flask
3. 1L beaker
4. Hot plate
5. Magnetic stirrer
6. Syringe
7. Weighing balance
8. Filter paper
9. Filter tunnel
10. Spatula
11. Crucibles

Recommended/Suggested Literature:

1.Mullin J. W., Crystallisation, Butterworth Heinemann.

2. Mengying Tao, Zhao Wang,*Junbo Gong, Hongxun Hao, and Jingkang Wang,
Determination of the Solubility, Dissolution Enthalpy, and Entropy of Pioglitazone
Hydrochloride (Form II) in Different Pure Solvents, Ind. Eng. Chem. Res. 2013, 52,
30363041
3. Siti Kholijah Abdul Mudalip, Mohd. Rushdi Abu Bakar, Fatmawati Adam, and Parveen
Jamal Solubility and Dissolution Thermodynamic Data of Mefenamic Acid in Different
Classes of Organic Solvents J. Chem. Eng. Data, 2013, 58 (12), pp 34473452.

4. F., Adam; A. B., Siti Hana; Yusoff, Mashitah M.; S. N., Tajuddin, Molecular Dynamic
Simulation of The Patchouli Oil Extraction Process, J. Chem. Eng. Data, 2014, 59 (2), pp
183188.

5. Siti Kholijah Abdul Mudalip, Mohd. Rushdi Abu Bakar, Fatmawati Adam, and Parveen
Jamal, Structures and Hydrogen Bonding Recognition of Mefenamic Acid Form I
Crystals in Mefenamic Acid/Ethanol Solution, International Journal of Chemical
Engineering and Applications, Vol. 4, No. 3, June 2013

Fatmawati Adam/ Jolius Gimbun

 EXPERIMENT 2: THIN FILM EVAPORATOR

OBJECTIVE
1. To demonstrate the evaporation of ethanol - propanol mixture
2. To determine effect of heating temperature and vacuum pressure on the
evaporation rate.

INTRODUCTION
The thin film evaporation unit is a complete evaporation system including feed input,
heating and vacuum generation for continuous plant operation. The unit is 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 adopts a
rotating film system, where molecules are continuously evaporating from a film which
is spread by a rotating wiper.

EQUIPMENT/APPARATUS/MATERIAL
1. BP215 Thin Film Evaporator
2. Stop watch
3. Beakers
4. Refractometer
5. Cooling Water Supply
6. Ethanol
7. Measuring Cylinder
8. Propanol

EXPERIMENTAL PROCEDURES
1. Prepare a set of mixtures containing ethanol and propanol within a specified
range of composition between pure ethanol and pure propanol.
Determine refractive index (RI) for each mixture using a refractometer.
2. Prepare 10L of ethanol-propanol mixture at a composition at composition
60:40 v/v. Obtain a sample from the feed liquid at valve V2 and analyze
the sample to determine its actual initial composition.
3. Perform the general start-up procedures with the following default settings:
metering pump P1 : 60% stroke, 60 stroke/min
heating thermostat T1: 60C
vacuum controller PIC-1 : 400 mbar
4. Allow the unit to run for about 5-10 minutes to achieve steady state. Steady
state is reached when the distillate temperature doesnt change
significantly over time.
5. Record the distillate temperature.
6. Measure the distillate and bottom product flow rates.
7. Collect the product from both distillate and bottom product vessels B2 and B3.
Analyze the collected liquid to determine its compositions
8. Repeat the experiment by reducing the vacuum pressure down (Range 750
350 mbar).
9. Return the vacuum pressure to default. Repeat the experiment by increasing
the heating thermostat up (Maximum 90C).

Fatmawati Adam/ Jolius Gimbun

 RESULTS

Initial Feed Composition :

P1 : 60% stroke, 60 stroke/min

No Heating Vacuum Distillate Bottom Product

Temp. Pressure
C mbar
Temp Flow RI Composition Flow rate RI Composition
C rate mL/min
mL/min
Constant Temperature at 60C (Setting at T1 = 75C)
1 60
2 60
3 60
Constant Pressure at 500mbar
4 500
5 500
6 500

*Use Antoine Equation to determine the right temperature/pressure setting

Log10P = A- B/(C+T)
Antoine Constant [Temperature in C and Pressure in mmHg)

Component A B C TMin[C] TMax[C] Psat[mmHg]

8.1122 1592.864 226.184 20 93 1693.832048
Propanol 7.74416 1437.686 198.463 60 106 845.657321
Propanol 8.37895 1788.02 227.438 -15 98 828.5394222

**Temperature setting at T1 should be 15oC higher than calculated temperature due

to heat loss.

Fatmawati Adam/ Jolius Gimbun

Fatmawati Adam/ Jolius Gimbun
Fatmawati Adam/ Jolius Gimbun
 EXPERIMENT 3: SHORT PATH DISTILLATION

OBJECTIVE
Study on the effects of the parameters on the thermal separation efficiency using
short path distillation

SCOPE
To study the effects of stirrer speed and temperature on the efficiency of ethylene
glycol-water separation in a short path distillation

INTRODUCTION
This Short Path Distillation is a thermal separation process for thermal sensitive
products. Short residence time and low evaporation temperature will cause a
minimum thermal stress to the distilled product. Typical applications are high
molecular organic compounds particularly from the field of chemistry, pharmaceutical
and food industry. Distillation is one of the most important thermal separation
methods.

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 evaporation 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 vapours on their way 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 condenser

EQUIPMENT/APPARATUS/MATERIAL
1. Short Path Distillation Unit
2. Ethylene glycol water mixture

EXPERIMENTAL PROCEDURES

1. Mix the ethylene glycol and water with a ratio of 5:5 at total of 1 litre in a
beaker. Then stir the mixture homogeneously.
2. Check that all valves are initially closed except the valves HV04, HV05, HV11
and HV12. Ensure that the cold trap is filled with dry ice.
3. Switch ON the main power supply at the control panel.
4. Set the thermostat at 70C, Chiller at 12C and vacuum pump pressure at 250
mbar. Manually maintain the pressure throughout the experiment. [To adjust
vacuum pump pressure, manually adjust valve, V14. To adjust the desired
stirrer speed, adjust knob button at stirrer].
5. Once the chiller temperature and thermostat temperature have reach the set
points, the equipment is ready for experiment.
6. ON feed pump and set it to 10 rpm and then ON stirrer (set to desired speed).
7. For every set of experiment, run for 5 minutes. After 5 minutes, records down
the volume of distillate from V-104 and volume of concentrate from V-105-
107.

Fatmawati Adam/ Jolius Gimbun

 8. Repeat the experiment with different operating parameters as shown in the
table in result and discussion.
9. Follow the operating procedure to shut down the equipment. DO NOT let the
wiper roller to run without the flow of feed.

GENERAL SHUT-DOWN PROCEDURES

1. Switch off vacuum pump.
2. Switch off feed pump and stirrer motor.
3. Turn off thermostat.
4. Open valve HV 06 and HV 07.
5. After 15 minutes, switch off chiller and turn off the main power.

NOTE: DO NOT attempt to remove any vessel while the vacuum pump is running.

RESULT
1. Effect of stirrer speed

Vacuum pressure, PT-200 100mbar

Evaporator Temperature, TT- 70C
100
Feed Flow rate ml/min
Contact time 5 min
EG-water ratio 7:3

Time Start Stirrer Distillate Concentrate Separation

Speed(rpm) Volume (ml) Volume (ml) Efficiency (%)
50
100
200
220

2. Effect of evaporator temperature

Feed flow rate ml/min

Stirrer speed, M-500 220rpm
Vacuum pressure 100mbar
Contact time 5min
EG-water ratio 7:3

Time Start Temp (C) Distillate Concentrate Separation

Volume (ml) Volume (ml) Efficiency (%)
70
72
74
76
80

Fatmawati Adam/ Jolius Gimbun

Fatmawati Adam/ Jolius Gimbun
 EXPERIMENT 4: SIEVE TRAY DISTILLATION

OBJECTIVE
1. To determine the height equivalent theoretical plates (HETP) at total reflux.
2. To determine the effect of liquid and vapor loading on the HETP at total reflux.

INTRODUCTION
The principle for sieve tray distillation is the same as for normal distillation: when a
liquid mixture is heat so that it boils, the composition of the vapor above the liquid
differs from the liquid composition. If this vapor is then separated and condensed into
a liquid, it becomes richer in the lower boiling component(s) of the original mixture.
This is what happens in a sieve tray distillation column. A mixture is heated up, and
routed into the distillation column. On entering the column, the feed starts flowing
down but part of it, richer in lower boiling component(s), vaporizes and rises.
However, as it rises, it cools and while part of it continues up as vapor, some of it
(enriched in the less volatile component) begins to descend again.

Figure 1: shows a simple continous fractional distillation tower for separating a feed
stream into two fractions, an overhead distillate product and a bottoms product. The
lightest products (those with the lowest boiling point or highest volatility) exit from
the top of the columns and the heaviest products (the bottoms, those with the
highest boiling point) exit from the bottom of the column. The overhead stream may
be cooled and condensed using a water-cooled or air-cooled condenser. The
bottoms reboiler may be a stream-heated or hot oil-heated heat exchanger, or even
a gas or oil-fired furnace. In a continous distillation, the system is kept in a steady
state or approximate steady state. Steady state means that quantities related to the
process do not change as time passes during operation. Such constant quantities
include feed input rate, output stream rates, heat and cooling rates, reflux ratio, and
temperatures, pressures, and compositions at every point (location). Unless the
process is disturbed due to changes in feed, heating, ambient temperature, or
condensing, steady state is normally maintained. This is also the main attraction of
sieve tray distillation, apart from the minimum amount of (easily instrumentable)
surveillance; if the feed rate and feed composition are kept constant, product rate
and quality are also constant. Even when a variation in conditions occurs, modern
process control methods are commonly able to gradually return the sieve tray
process to another steady state again.

EQUIPMENT/APPARATUS/MATERIAL
1. Sieve Tray Distillation Unit
2. Refractometer
3. 7L of binary mixture (ethanol-propanol)
4. Beakers

EXPERIMENTAL PROCEDURES
1. Prepare a set of mixtures containing ethanol and propanol within a specified
range of composition between pure propanol and pure ethanol. Determine
refractive index (RI) for each mixture using a refractometer.
2. Ensure all valves are closed.
3. Prepare a mixture of ethanol and propanol at desired composition (for
instance 5 L mixture containing 3 L of ethanol and 2L of propanol).

Fatmawati Adam/ Jolius Gimbun

 4. Record initial volume and refractive index of the liquid mixture.
5. Open the charge port cap and charge the reboiler B1 with the ethanol-
propanol mixture. Close the charge port cap.
6. Make sure all the valve are properly close except V15 and V14 for cooling
purposes.
7. Turn on the main power on the control panel.
8. Ensure the reflux control is 0 position(total reflux)
9. 9. Switch on the cartridge heaters W1 and set the heater power regulator to
1.0 kW and allow the reboiler temperature reach approximate 85C.
10. 10. As the top column temperature sensor TT 112, reach steady state, record
the temperature.
11. 11. Set the reflux control to position 1(Total distillate offtake). When the level
in phase separator reaches 100mL, start the timer. As distillate reach 200mL,
stop the timer and determine the flowrate of the distillate.
12. 12. Open valve V9 and collect sample distillate using beaker. Close valve V9
and set the reflux control to position 0 (Total reflux).
13. 13. To collect bottom product sample, open valve V8 and V2 to collect 10 ml
of sample bottom product using beaker. Close valve V2 & V8.
14. 14. Measure the refractive index of the samples and record the value into data
table.
15. 15. For different liquid and vapor loading, adjust the heater power settings in
W1 according table below:

Heater Power
(kW)
1.00
1.50
2.00

16. Wait for approximately 5 minutes and allow the distillation unit to achieve new
steady state. Repeat steps 9 to 13.
17. Switch off heater power and allow the system to cool down to ambient
temperature.

RESULT
Table 1: Data Collection for Distillate and Bottom Product
Heater Distillation Bottom Product HETP
W1, W2 (mm)
Temp Refractive Mole Temp Refractive Mole
Power
(C) Index Fraction (C) Index Fraction
(kW)
1.00
2.00
3.00

Fatmawati Adam/ Jolius Gimbun

EXPERIMENT 5: SOLID LIQUID EXTRACTION

OBJECTIVE
1. To study the salt extraction from sea-shore sand using solid-liquid extractor
unit.

INTRODUCTION
Separation processes are a fundamental part of almost every chemical process.
Indeed, there are usually far more separation stages in the overall process than
there are chemical reactions. Separations start with the extraction. Solid-liquid
extraction can be defined as the removal of one or more components from a solid
phase (or mixture of phases) by using a liquid to selectively dissolve the required
fraction. Generally, the process can be considered in two steps:
Contact of solid with liquid and selective dissolution of one or more
components of the solid phases.
Separation of the resulting solution from the residual solid.

EQUIPMENT/APPARATUS/MATERIAL

1. CTS6 Solid Liquid Extraction Unit 7. Sand (from sea-shore) as the solid
2. Steam supply 8. Table salt (50g)
3. Portable Conductivity Meter 9. Six 250mL beakers
4. Stop watch 10. 100mL graduated cylinder
5. Digital balance 11. 2L measuring jug
6. Tap water as solvent

EXPERIMENTAL PROCEDURES
1. Prepare standard salt solution and get its conductivity by using conductivity
meter.
2. Solid charging
Weigh out the appropriate quantity of solids into the fibre bag (typically 2
kg).
Carefully remove the solvent food line and vent line fitted to extraction
vessel cover.
Open extraction vessel cover and place the fibre bag containing the solids
into the extraction vessel, ensuring that the top of the bag is open for
downward solvent flow.
Replace the vessel cover and hand tighten the securing clips.
Replace the vent and solvent food lines.
3. Solvent charging
Open charge valve V4.
Fill the water carefully until its reach the level of the vessel equator.
4. Extraction by continuous downward displacement.
Ensure that the solvent feed line from below the distillate cooler is firmly
attached to the top of the extraction vessel.
Close V5.

Fatmawati Adam/ Jolius Gimbun

 5. Start up this equipment by follow General Start Up Procedures - Pre Start Up
Checks; Start-up Circuit 1 Cooling Water; and Start-up Circuit 3 Heating in
Work Instruction (attached on equipment).
6. 15 minutes after solvent has begun to pass through the product cooler,
measure the flowrate FI 1 and adjust the heat input to give a flowrate of
approximately 500ml/min. To measure the solvent flowrate, follow this step:
Set the equipment for return of solvent to reboiler section by close valve
V5.
When the solvent reaches the bottom mark on FI 1 begin timing and stop
the timing when the solvent reaches the top mark of FI 1.
Open valve V5.
7. When a steady value for FI 1 has been determined, records its value its value
and the values indicated by TI 1 and PI 4.
8. Carefully take a sample from the reboiler by open sampling valve V2 and
remove sample. Close V2 when sample is removed.
9. Close valve V5 and begin solvent transfer to the extraction vessel.
10. Take a sample of the first effluent:
Close stop valve V8.
Carefully open sampling valve V3 and remove sample. Close sampling
valve V3.
Open stop valve V8.
11. Record the collection of this sample as T=0.
12. Sample reboiler contents and effluent every 2 minutes for the first 10 minutes,
then every 5 minutes until 30 minutes then at T=45.
13. Record the final temperature indicated by TI 1.
14. Determine the conductivity for each sample taken.
15. Shutdown the equipment by following the instruction in part of General Shut
Off Procedures in Work Instruction.

Fatmawati Adam/ Jolius Gimbun

RESULT

Experimental Data

Weight of solid charge : TI 1 (Final) :

FI 1 : PI. 4 :
TI 1 (Initial) :

Time Reboiler Effluent

(min) Conductivity Salt Conc. g/L Conductivity Salt Conc. g/L
0
2
4
6
8
10
15
20
25
30
35
40

Fatmawati Adam/ Jolius Gimbun

EXPERIMENT 6: ABSORPTION COLUMN UNIT

OBJECTIVE
To study gas absorption in absorption column

Scope
1. To determine the effect of air flow rate and water flow rate on flooding point in
an absorption column.
2. To explain the relationship between water and air flow rate changes and their
effect on pressure drop, P of an absorption column.

INTRODUCTION
Absorption column is one of the separation techniques that involve liquid and vapor.
One or more component of a gas mixture can be separated when a certain liquid
flow through it counter-currently. The liquid absorbs the component(s) and mass
transfer process which separates the component(s) from gas mixture occurs. Packed
material is used to increase the contact surface area in absorption process which
enhances the efficiency and shortens the duration of the process.

EQUIPMENT/APPARATUS/MATERIAL
1. Packed Absorption Column
2. Air Compressor
3. Water and Air
4. Stop watch

EXPERIMENTAL PROCEDURES
1. Check and make sure the valves for right column for sadle pack are opened.
2. Set the water flow rate at 2.5 L/min.
3. Set the air flow rate at 100 L/min. Start the stop watch and leave it for 5
minutes. Make sure the water and air flow rate are always constant.
4. After 5 minutes, take the data for pressure drop, P from Digital P Meter.
5. Repeat Steps 3 and 4 by increasing air flow rate by 10 L/min until the flooding
point is observed.
6. When the flooding point is achieve, read the P from Digital P Meter and
reduce the air flow rate back at 100 L/min
7. Repeat Step(s) 3 to 7 for water flow rate at 3.0 L/min respectively.
8. Then, maintain the air flow rate at 100 L/min and, read the pressure drop
every 2 minutes at different water flow rates range from 2.0 to 3.5 L/min with
an increment by 0.5 L/min

Fatmawati Adam/ Jolius Gimbun

RESULT

Table 1
Water flow rate, Air flow rate, G Pressure Drop, Time
W (L/min) P (every 5
(L/min) (cm H2O) minutes)
2.5

3.0

Table 2
Air flow rate, G Water flow rate, Pressure Drop , Time
(L/min) W P (every 2
(L/min) (cm H2O) minutes)
2.0
100 2.5
3.0
3.5

Fatmawati Adam/ Jolius Gimbun

EXPERIMENT 7: PRESSURE SWING ADSORPTION

OBJECTIVE
1. To study O2 adsorption from a gas stream using an adsorber filled with
sample carbon molecular sieve.
2. To plot the breakthrough curves using adsorption data.

INTRODUCTION
Gas adsorption is a process in which one or more components from a gas stream
are adsorbed on the surface of a solid. Separation is accomplished because
differences in molecular weight, shape, or polarity give rise to some molecules being
held more strongly on the surface than others or because the pores are too small to
admit the larger molecules.

The solid that take up the gas is called the adsorbent, and the gas taken up on the
surface is called the adsorbate. Many adsorbents are highly porous materials, and
adsorption takes place mainly on the walls of the pores or at specific sites inside the
particle. In most applications, the adsorbing component (or adsorbate) is held
strongly enough to permit complete removal of that component from the fluid with
very little adsorption of other components. Regeneration of the adsorbent can then
be carried out to obtain the adsorbate in nearly pure form.

In this experiment, the Pressure Swing Adsorption (PSA) technology is used to

separate some gas species from a mixture of gases under pressure according to the
species' molecular characteristics and affinity for an adsorbent material. It operates
at near-ambient temperatures and so differs from cryogenic distillation techniques of
gas separation. Special adsorptive materials (e.g.carbon molecular sieve) are used
as asborbent, preferentially adsorbing the target gas species at high pressure. The
process then swings to low pressure to desorb the adsorbent material.
A plot of the outlet concentration with respect to time is called the breakthrough
curve as shown in Figure 1.

Figure 1: Breakthrough curve

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The S-shaped mass transfer region moves along the bed with time as the fluid
continues to flow. At times t1, t2 and t3, the exit concentration is practically zero. It
remains zero until the mass transfer zone starts to reach the end of the bed at a time
before t4. Then, the outlet concentration starts to rise until it reaches some limiting
permissible value, or break point. The break point concentration, cb, represents the
maximum allowable concentration of the outlet fluid, and is often taken as a relative
concentration, c/c0of between 0.01 to 0.05.

After the break point is reached, the relative concentration rises very rapidly until
time t*, then more slowly approaching cd, which is the end of the breakthrough curve
where the adsorption bed is considered ineffective. The value for cd is usually equal
to the feed concentration,c0.

It can be shown that the area between the curve and the c/c0 line at 1.0 is
proportional to the total solute adsorbed if the entire bed reaches equilibrium with the
feed. The ideal adsorption time for a vertical breakthrough curve is taken at time t*,
in which the rectangular area to the left of t* is proportional to the amount adsorbed.
For a symmetrical curve, t* is the time when c/c0 reaches 0.5.

EQUIPMENT/APPARATUS/MATERIAL

1. SOLTEQ Pressure Swing Adsorption Unit (Model: BP202A)

2. Carbon Molecular Sieve
3. Nitrogen Gas
4. Air

EXPERIMENTAL PROCEDURES

1. Check that all tubings are properly connected.

2. Ensure that V1 and V2 are closed.
3. Fill the column with the required adsorbent.
4. Turn on the power.
5. Ensure that the columns are regenerated prior to running any experiment by
following all the steps below:

a) Depending on which column to use, set valves to the following positions:

Valve K1 K2
desorption desorption
V1 Closed Closed
V2 Opened Opened
SV1 OFF ON
SV2 OFF ON
SV3 ON ON
SV4 OFF ON

b) Supply N2 gas to the pipeline

c) Open and adjust pressure regulator to 2.0 bar.
d) Open valve V2 and adjust flowmeter for OT2 at 0.5LPM.

Fatmawati Adam/ Jolius Gimbun

 e) Turn off the N2 supply when OT2 analyser shown 0%.

6. Now, the unit is ready for experiment.

7. Unplug N2 gas supply and plug in compress air where adjust the pressure
regulator to 0 bar (anticlockwise).
8. Record the result by using DAS (Data Acquisition Software) and turn on the
pressure regulator (clockwise) until 2 bars to start the experiment.
9. Continue collecting samples until the oxygen sensor reading are constant.
10. Repeat step 1 to 13 by using different flowrate and pressure.
NOTE: Make sure that the column has been regenerated before use.

GENERAL SHUT-DOWN PROCEDURES

1. Switch off the vacuum pump or compressor.
2. Turn off the power for the control panel.
3. Close all valves for the gas supply lines.

RESULT

Pressure Flowarate Time (s) Inlet Outlet

(bars) (L/min) concentration concentration
of Oxygen, c of Oxygen, c
2 30 t = 0 to
breakthrough
2 40
3 30
3 40

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 Figure 4: Process flow diagram for the pressure swing adsorption BP202A unit

FORMULAS

1. Molarity = Mole / Liter

= (Specific Gravity x Purity x 1000mg/L) / Molecular Weight
2. Mole = Mass / Molecular Weight
3. M1V1

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