LABORATORY

MODULE

PTT 356/3
SEPARATION ENGINEERING
SEMESTER 1 (2019/2020)

Dr. Mohd Sharizan Md Sarip

Dr. Siti Kartini Enche Ab Rahim
Dr. Azduwin Khasri
Dr. Amira Mohd Nasib
Pn. Nor Aida Binti Yusoff
Pn. Nur Zatul ‘Iffah Binti Zakaria
Cik Rumaisa Nordin
En. Mohd Qalani Che Kasim

Department of Chemical Engineering Technology

Faculty of Engineering Technology
University Malaysia Perlis

1
 TABLE OF CONTENTS

CONTENTS PAGE

EXPERIMENT 1: YIELD AND EFFICIENCY DETERMINATION FOR 1

LIQUID-LIQUID EXTRACTION PROCESS

EXPERIMENT 2: YIELD AND EFFICIENCY DETERMINATION FOR 6

SOLID-LIQUID EXTRACTION PROCESS

EXPERIMENT 3: YIELD AND EFFICIENCY DETERMINATION FOR 14

CRYSTALLIZATION PROCESS

EXPERIMENT 4: YIELD AND EFFICIENCY DETERMINATION FOR 20

CENTRIFUGATION PROCESS

EXPERIMENT 5: YIELD AND EFFICIENCY DETERMINATION FOR 24

MEMBRANE SEPARATION PROCESS

EXPERIMENT 6: EFFECT OF REGULATING REFLUX RATIO ON TOP 29

PRODUCT COMPOSITION IN DISTILLATION PROCESS

APPENDICES 35

2
Guidelines for Writing Laboratory Report
PTT356 – Separation Engineering

 Use the given laboratory report format as given by the instructors.

 All report must be typed in word and printed out for submission.
 Use Arial as the font with a font size of 8-12.
 All data sheets must be included as the appendix of the report.
 All report must be done in past tense, with the exemption of grammatical rules
for a certain sentences. For methodology, full sentence with passive voice
must be used.
 All results, tables, graphs, figure, etc, must be done using computer software
(e.g. Microsoft Excel, Word, Origin, Aspen HYSYS, etc.). However, for a certain
graphs that require hand drawing skill, manual plotting is acceptable.
 The maximum number of page of each report is 8 PAGES (the front page and
appendix). Anything after page 8 (except the appendix) WILL NOT be read,
marked and hence, evaluated.
 Each laboratory report must consist of:
o Front cover
o Objective
o Introduction and Methodology
o Results
o Discussion
o Conclusion
o Reference
 Marks will be given based on:
o Report submission punctuality
o Organization & format
o Language
o Objective
o Intorduction and Methodology
o Results
o Discussion
o Conclusion
o References
o Plagiarism
 Plagiarism will not be tolerated. Any suspicion on plagiarism would be
investigated and if found guilty, resulted in zero mark for that submitted
laboratory report and a barred access to the subsequent lab session.

3
 EXPERIMENT 1
YIELD AND EFFICIENCY DETERMINATION FOR LIQUID-LIQUID EXTRACTION
PROCESS

1.0 OBJECTIVES
1.1 To demonstrate the liquid-liquid extraction process.
1.2 To determine the height equivalent theoretical plates (HETP) for the column.
1.3 To calculate and analyze the efficiency of the liquid-liquid extraction process.

2.0 INTRODUCTION
The Liquid-Liquid Extraction Unit (Model: BP 61) has been designed to
demonstrate the basic principles of a liquid-liquid extraction process. In a normal
operation, the light and heavy phase liquids are pumped counter-currently into the packed
extraction column. The heavy phase will enter at the top of the column and flow downwards
while the light phase will enter at the bottom of the column and flow upwards due to density
differences. Countercurrent flow among the packings in the column of these two phases
will cause the transfer of solute component from one phase (raffinate) to the other (extract).
The raffinate will emerge at the bottom while the extract will emerge at the top of the
extraction column. This liquid-liquid extraction process is carried out among the column
packings to give a higher degree of separation. Sampling points are provided at key
positions around the unit to allow collection of both light and heavy phase liquids. In this
way, the effects of feed flow rates of both phases on the extraction efficiency can be
evaluated by means of sample analysis.

3.0 THEORY
When separation by distillation is ineffective, liquid-liquid extraction is one of the
main alternatives to consider. Close boiling mixtures or substances that cannot withstand
the relatively high temperature of distillation, even under a vacuum, may often be
separated from impurities by the mean of extraction, in which utilizes
chemical/concentration differences instead of vapor pressure differences. Separation by
liquid-liquid extraction can be defined as the selective removal of one or more
components either from a homogeneous liquid mixture or from a solution, using a
second liquid or solvent, which is partially or wholly immiscible with the first. Figure
2.1 illustrates the typical terms used to describe the different streams in a liquid-liquid
extraction system.

Figure 2.1. Flow of streams and components in a liquid-liquid extraction system.

In an extraction process, a quantity of feed liquid, F is mixed with a quantity of

solvent, S in an agitated vessel. After which the layers are settled and separated, the
extract may be lighter or heavier than the raffinate. As such, it may be shown coming from
the top of the equipment in some cases and from the bottom in others. Since the feed is a
two component system, by convention, the material to be extracted is commonly referred
to as the solute while the other component is generally referred to as the diluent. The
raffinate stream has the same components as the feed, though the proportions are
different, with the raffinate having a much lower solute concentration. An ideal unit with

1
perfect extraction will yield a raffinate which has only one component, that being pure
diluent. The liquid used to strip the solute from the feed is referred to as the solvent.
However, solvent is a general term and should not be confused with the feed solvent or
diluent. The solvent after becoming enriched in solute leaves the system as the extract.

Since the liquid-liquid extraction involves a 3-component system, a graphical

representation of the liquid mixtures is usually employed. There are two graphical systems,
namely: Rectangular coordinates and Triangular coordinates. The rectangular
coordinates are easier to plot, but the triangular coordinates offer a more representative
view of the component compositions. However, it is important to fix the basis for the
representation before doing any calculations. This manual will assume a composition basis
of mole fraction and plots all component compositions in triangular coordinates (Figure
2.2).

Figure 2.2. A typical 3-component system representation on an equilateral triangular

diagram (A = solute; B = diluent; C = solvent)

The assignment of symbols are arbitrary. Confusion shall not arise as long as the
apex for the solute is at the top while the bottom apexes are for the solvent and diluent.
Referring to Figure 2.2, the curve on the triangular diagram is called the binodal or
solubility curve of the ternary system. The curve, which is essentially a combination of
diluent-rich and solvent-rich curves, separates the upper region of stable single phase
mixture from the lower region of unstable mixture, which tends to separate into two phases.

The compositions of extract, E and raffinate, R are connected by tie-lines having

different slopes (i.e. not parallel). The tie lines get shorter as they get away from the x-
axis, and eventually they converge at a point P (plait point). The point P is not normally the
highest part of the curve. The number of theoretical stages can be determined graphically
by constructing operating lines and tie-lines on the binodal/solubility curves, as outlined in
Figure 2.3. Consequently, the effects of different stirrer speeds and feed flow rates on the
extraction efficiency can then be evaluated.

2
 Figure 2.3. Operating lines and tie lines constructions for determination of extraction
efficiency.

4.0 MATERIAL AND EQUIPMENT

4.1 SOLTEQ liquid-liquid extraction unit (Model: BP61)
The liquid-liquid extractor is designed for the demonstration of liquid mixture
separation by solvent extraction process, as portrayed in Figure 2.4 and Table 2.1.
All glass components of the extraction unit are made of borosilicate 3.3 glass with
PTEE gaskets.

Figure 2.4. Liquid-liquid extraction unit.

Table 2.1. Description of each components

1. Feed tank (B1/B2) Graduated cylindrical vessels with 20 L
capacity.
2. Extraction column A DN50 packed column with 10 mm ceramic
(K1) berl saddles. Effective height of column is 1.5
m.
3. Metering pumps (P1) Chemical dosing pumps with up to 36 L/h
capacity.

3
 4. Metering pumps (P2) Chemical dosing pumps with up to 18 L/h
capacity.
5. Product tanks Graduated cylindrical vessels with 20 L
(B3/B4) capacity.

4.2 List of Materials

(i) Distilled water
(ii) Acetone
(iii) Toluene

4.3 List of Apparatus

(i) Refractometer
(ii) Measuring cylinders
(iii) Beakers
(iv) Dropper
(v) Tissue papers

5.0 PROCEDURES
5.1 Safety Considerations and Maintenance
5.1.1 The unit must be operated under the supervision of an authorized staff who
has been properly trained to handle the unit.
5.1.2 All operating instructions supplied with the unit must be carefully read and
understood before attempting to operate the unit.
5.1.3 Feed stock which severely affect Stainless steel, PTFE, PE and borosilicate
glass are not to be used.
5.1.4 The system should not be subjected to shock, sudden impact, vibration,
additional load, or permanent external action of aggressive vapors.
5.1.5 Always check and rectify any leak.
5.1.6 Be extremely careful when handling hazardous, flammable or polluting
materials.
5.1.7 Restore the system to operating conditions after any repair job.
5.1.8 Make sure the system is sufficiently ventilated when working at atmospheric
pressure.
5.1.9 Only a properly trained staff shall be allowed to carry out any servicing.
5.1.10 Before any servicing, shut down the whole operation and let the system to
cool down and be properly ventilated.
5.1.11 Do not use any coarse or abrasive cleaners on glass components.
5.1.12 Leaking couplings should be carefully retightened. Replace any gaskets or
seals if necessary.
5.1.13 Make sure to rinse the tanks, flow sensors and pumps with distilled water
after any usage or experiments.
5.1.14 Make sure there is no leakage on the tubing, failure to do so will cause the
flow sensor to show no reading due to air bubble inside the turbine.

5.2 General Start-Up Procedure

5.2.1 Prepare the following chemicals:
(a) Feed: mixture of acetone-water solution at the desired composition (e.g.
40 %v/v of acetone).
(b) Solvent: pure toluene
5.2.2 Ensure that all valves are closed.
5.2.3 Fill feed tank B2 with 10L of acetone-water solution and feed tank B1 with
10L of pure toluene solvent.
5.2.4 Turn on the main power at control panel.

4
 5.2.5 Switch on pump P2. Allow the acetone-water solution to enter the column
and fill to a level of about 5-15 cm above the solvent inlet.
5.2.6 Switch on solvent pump P1.
5.2.7 As the solvent enters the column, carefully watch the interface level which
forms between the light and heavy phases.
5.2.8 Once the liquid starts to overflow at the top of the column, stops pump P1
and P2.
5.3 Experimental Procedure
5.3.1 Perform the general start-up procedure.
5.3.2 Start both pumps P1 and P2 and set the desired feed and solvent feed flow
rates by adjusting the pump speed (e.g. feed flow rate 0.2 L/min and solvent
flow rate is 0.18 L/min).
5.3.3 Allow both liquids to flow into the collection vessel B3 and B4 respectively.
The bottom product contains the water rich phase (raffinate) while the top
product contains the toluene rich phase (extract).
Note: Monitor the interface level. Maintain the interface level above the solvent inlet
by adjusting the height of the overflow tube, or switching off pump P1 temporarily.
5.3.4 Let the experiment run for a while to attain steady state.
5.3.5 Open valve V5 to collect a 10 mL sample of raffinate and open valve V2 to
collect a 10 mL sample of extract for every 5 minutes until 60 minutes.
5.3.6 Record the refractive index of both samples using Appendix 1.

5.4 General Shut-Down Procedure

5.4.1 Open valves V1, V3, V4, V5, and V6 to drain all liquid from the equipment.
5.4.2 Fill the solvent tank B1 and feed tank B2 with distilled water.
5.4.3 Switch on pumps P1 and P2 for about 10 minutes to rinse all the remaining
solution in the tanks, flow sensors and extraction column.
5.4.4 Drain all the liquid from the equipment by opening the valve V1, V3, V4, V5,
and V6.
5.4.5 Switch off pumps P1 and P2 and turn off the power of the control panel.

6.0 RESULTS
6.1 Record your result into a table as in Appendix 1.
6.2 Plot a graph to show the extraction profile.
6.3 Develop a mass balance calculation for the extraction process to obtain the extract
and raffinate flow rates.
6.4 Determine the required theoretical extraction stage from the liquid-liquid extraction
experiment results (refer Appendix A1-A4).
6.5 Calculate the height equivalent theoretical plates (HETP) of the extraction column.
HETP = Effective column height / No. of theoretical plate
6.6 Calculate the separation efficiency.
Efficiency = Amount of extracted solute / Amount of solute in feed

7.0 DISCUSSION
7.1 Sketch the process flow diagram for this experiment.
7.2 Discuss the finding of the graph and result.
7.3 Predict and discuss the effect of regulating solvent flow rate on the percentage of
acetic acid recovered in the extract stream.
7.4 Discuss any discrepancies and sources of error that influence the reproducibility of
the experimental result.

8.0 CONCLUSION
Based on the experimental procedure done and the results obtained, draw some
conclusions to this experiment.

5
 EXPERIMENT 2
YIELD AND EFFICIENCY DETERMINATION FOR SOLID-LIQUID EXTRACTION
PROCESS

1.0 OBJECTIVES
1.1 To demonstrate the solid-liquid extraction process.
1.2 To investigate the effect of contact time and solvent temperature on the solid-liquid
extraction process.
1.3 To calculate and analyze the efficiency of extraction process.

2.0 INTRODUCTION
Separation processes by extraction are a fundamental part of almost every
chemical process. Separations start with the extraction of raw materials and continue to
the purification and isolation of the final product. In a solid-liquid extraction process, one
or more components from a solid phase (or mixture of phases) can be removed by using
a liquid (solvent) to selectively dissolve the required solute.

3.0 THEORY
3.1 Definitions and Nomenclature
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 solute fraction. A complete extraction generally
includes the following three steps:

a) Contact of solid with liquid and selective dissolution of one or more components
of the solid phases.
b) Separation of the resulting solution from the residual solid.
c) Separation of the solute from the solvent in the extracted solution.

Solid-liquid extraction can be used either when the extracted component is

required or to recover the solid residue. The former is generally described as
leaching, while the latter is more often associated with purification such as washing
of filter cakes. The solvent feed (extractant) is allowed to come into intimate contact
with the solids feed. The resulting solution (solute and solvent), which leaves the
process, is described as the overflow (effluent stream), while the residual solid (inert)
together with the entrained solution make up the underflow.

Throughout this experiment, the following naming conventions will be used:

A = solute; B = inert or leached solids; C = solvent; V and x refers to the flow rate
and composition of the overflow (effluent); L and y refers to the flow rate and
composition of the underflow (solid slurry).

3.2 Continuous Multistage Countercurrent Extraction

Figure 3.1 outlines the overall operation and naming convention of a multi
stage solid-liquid extraction operation. The ideal stages are numbered in the direction
of the solids and underflow stream. The solvent-solute phase (V), is the liquid phase
that overflows continuously from stage to stage counter-currently to the solid phase,
and it dissolves solute as it moves along. The slurry phase (L) composed of inert
solids and a liquid phase of entrained solution is the continuous underflow from each
stage. Note that the composition of the V phase is denoted by x and the composition
of the L phase by y, which is reverse for that of liquid-liquid extraction.

6
 Figure 3.1. Continuous multistage solid-liquid extraction.

In solid-liquid extraction, sufficient solvent is provided to dissolve all the solute

in the entering solid and there is no adsorption of solute by the solid, equilibrium is
attained when the solute is completely dissolved and the concentration of the solution
formed is uniform. In equilibrium system, the concentration retained by the solid
leaving any stage is the same as that of the liquid overflow from the same stage. The
equilibrium relationship is simply: xe = y.

In general, the equilibrium is given in the triangle diagram as shown in Figure

3.2. Solvent B and extractable solvent are completely miscible and therefore it is a
system with two mixing gaps. The connodes have to go through point A because
extract and solution in the solid particles have the same composition so that the ratio
C/B is constant. The minimum amount of the solvent is the coming closer of the
mixing point to the bimodal curve because all connodes cross in point A.

Figure 3.2. Equilibrium in the triangle diagram for solid-liquid extraction.

3.3 Efficiency
The efficiency of a solid-liquid extraction process can be defined in a number
of ways as described below. In general, all these efficiency values can be used to
compare between different operational techniques.

(a) Recovery (Overall Efficiency)

The recovery (otherwise known as process efficiency, overall efficiency, total
efficiency or degree of extraction) describes the amount of material removed from
a fixed mass of solid feed.

Recovery = Mass of component removed / Total initial mass of component

7
 (b) Recovery of more than one component
If not all of the mass of the material being extracted is available then it is possible
to define the effective recovery of each individual component.

Recovery of component – i = Mass of component i removed / Initial mass of

component i

(c) Yield
As a variant for the recovery of any component, yield of the component can also
be expressed as follows:

Yield = Mass of component removed / Total mass of feed

(d) Effective Recovery

If not all of the mass of the material being extracted is available, then it is possible
to define the effective recovery:

Effective Recovery = Mass of component i removed / Available mass of

component i

(e) Volumetric Recovery

If It is also important to consider the amount of solvent used in the recovery, the
volumetric recovery can be calculated:

Volumetric Recovery = Mass of component removed / Volume of solvent used

for recovery

3.4 Flowmeter Reading Conversion

The flow meter shows only the length of the meter. It uses water as its
reference point. To convert the length of the flow meter to flow rate, mL/min, some
calculations are needed. As an example, for water, the 150 mm of the flow meter is
equivalent to 506 mL/min. Thus, the convert length to flow rates can apply the
following equation:

Flow rate, mL/min = (506 / 150) x D x L

where D is the solution’s density (g/mL), and L is the reading length (mm).

3.5 Density Measurement

The density of a specific solution can be obtained by using a specific gravity
meter. The specify gravity meter is a highly calibrated cylinder. Density can be
calculated by using the following formula:

Density, mL/min = (a – b) / 49.552

where a is the weight of solution + cylinder, b is the weight of empty cylinder, and
49.552 mL represent the volume of cylinder.

4.0 MATERIALS AND EQUIPMENT

4.1 SOLTEQ solid-liquid extraction unit (Model: BP40)
SOLTEQ solid-liquid extraction unit (Model: BP40) is a teaching unit comprising of
an extraction vessel, an evaporator vessel with electric heater, a packed column, a
solvent condenser, a product cooler, a pre-heater, and a collecting vessel, all
manufactured in borosilicate glass, as shown in Figure 3.3. The detailed description
for each component is given in Table 3.1.

8
 Figure 3.3: Solid-liquid extraction unit.

Table 3.1. Detail description for each component in solid-liquid extraction unit.
No. Component Description
7 L spherical evaporator vessel made of stainless
1 Reboiler (B1) steel. Electrical safety heating mantle (W1), 2 kW
with temperature and level switch.
DN50 x 1000 mm column made of borosilicate
2 Column (K1) glass. Packings: glass Raschig rings (8 mm x 8
mm).
Vertical coil heat exchanger DN50 made of
3 Condenser (W2)
stainless steel. Heat transfer area: 0.3 m2.
Product Cooler Vertical coil heat exchanger made of stainless
4
(W4) steel. Heat transfer area: 0.03 m2.
Receiver Vessel
5 5 L spherical vessel made of stainless steel.
(B3)
Cylindrical vessel made of borosilicate glass with 4
Extraction Vessel
6 L solid sample container. Made of stainless steel
(B2)
with porous support.
7 Pre-Heater (W3) 150 W cartridge heater with temperature control.
3 temperature measurement points (TI-101, TI-
102, TI-103).
Instruments and 2 temperature controller (TIC-101, TIC-103).
8
Controls 1 flow rate measuring point (FI-301).
1 pressure indicator (PI-201).
1 level controller (LIC-101).
9 Framework Stainless steel tube with clamps.
Allowable pressure: -1 to 3 bar in tube and -1 to 1
Operating bar in shell.
10
Conditions Allowable temperature: 180°C in tube and 150°C
in shell.
11 General Electrical: 230VAC / 1-phase / 50Hz / 10A.

9
 Requirements Water supply: laboratory water.
Height: 1.730 m
12 Overall Dimensions Width: 1.216 m
Depth: 0.608 m
4.2 List of Materials
(i) Ethanol
(ii) Peanut oil
(iii) Crushed peanut
(iv) Toluene

4.3 List of Apparatus

(i) Balance
(ii) Measuring cylinders
(iii) Beakers
(iv) Sampling vials with caps

5.0 PROCEDURES
5.1 General Start-Up Procedures
5.1.1 Ensure that all the valves are initially closed, then open all vent valves (V6,
V7, and V9).
5.1.2 Charge the reboiler B1 with ethanol solvent (8 L).
Note: Refer to the solvent safety data sheet for proper handling.
5.1.3 Ensure that all tubing are properly connected.
5.1.4 Run the cooling water through the product cooler W4 and condenser W2.
Note: Open the cooling water valve V15 and keep it open throughout the
experiment. Open the valve slowly to prevent a pressure surge to the cooling
system.
5.1.5 Switch on the heating system for the reboiler as follows:
a) Initially, close valve V12 to allow total reflux.
b) Switch on the main power supply on the control panel.
c) Adjust the temperature controller TIC-101 set point to a few degrees
above the boiling point of the solvent. In the case of ethanol, adjust to
85oC.
d) Switch on heater W1.
e) Observe the temperature rise in the reboiler.
f) Allow the system to reach steady state at total reflux.
Note: if the column starts to flood and liquid begins to accumulate above the reflux
separator, temporarily switch off the heater W1 until column conditions are back to
normal.

5.2 Calibration of Solute Composition

5.2.1 Prepare mixtures of peanut oil and ethanol in different compositions; vary
from 0 to 1 g oil/g solvent.
5.2.2 Use the recommended calibration volumes in the sample table in Appendix
A3. Use a basis of 100 g solvent.
5.2.3 For an example, for a sample of 0.1 g oil/g solvent.
a) Weigh 100 g of ethanol solvent in a beaker.
b) Weigh 10 g of peanut oil in another beaker.
c) Add the oil into the solvent to form a homogenous solution.
Note: Do this step quickly to avoid solvent evaporation as ethanol is volatile.
5.2.4 Measure the density of the calibrated solution.
5.2.5 Plot a calibration curve of density versus solute composition.
5.2.6 Use that calibration curve for further experiments.

10
5.3 Calibration of Solute Composition
All samples should be collected in sampling vials with caps to avoid excessive
evaporation of the solvent. The samples will be used for density measurements.
5.3.1 Effluent sampling
a) Place a sampling vial below valve V3.
b) Open valve V3 and collect approximately 50 mL of effluent in the
sampling vial.
c) Close valve V3.
5.3.2 Reboiler sampling
Note: Sample taken from the reboiler will be at the boiling point of the solvent and
must be handled with extra care.
a) Place a sampling vial below valve V1.
b) Open valve V1 and collect approximately 50 mL of reboiler content in
the sampling vial. Quickly close valve V1.
c) Cool the sample by immersing the vial in cold water.
5.3.3 Distillate sampling
a) Place a sampling vial below valve V11.
b) Open valve V11 and collect approximately 50 mL of distillate in the
sampling vial.
c) Close valve V11.

5.4 Charging of Fresh Solid

Fill the extraction vessel B2 with fresh solid whenever it is required in the experiment.
5.4.1 Screen some crushed peanuts to obtain solids of sizes between 2 mm and
4 mm. Weigh approx. 1000 g of the peanuts.
5.4.2 Charge the extraction vessel B2:
a) Ensure that the extraction vessel is drained of solvent.
b) Carefully remove the vessel cover and the solid container.
c) Discard any used solid in the container.
d) Fill the container with the screened peanuts.
e) Carefully place the container back into the extraction vessel.
f) Replace the extraction vessel cover.
5.4.3 Check that the solvent feed line is properly connected to the extraction
vessel.

5.5 Solvent Refill in the Reboiler

5.5.1 Switch off the heater W1.
5.5.2 Allow the solvent temperature in the reboiler to drop below boiling point and
observe until the boiling is stopped.
5.5.3 Open reboiler cap, quickly refill the reboiler to minimize escape of solvent
vapor. Immediately close valve reboiler cap.
5.5.4 Switch on the heater W1.
Note: DO NOT open reboiler cap while temperature in the reboiler is still boiling.

5.6 Experimental Procedure

5.6.1 Perform the general start-up procedures (Section 5.1). Check that all valves
are initially closed except the vent V6, V7 and V9. Ensure that the extraction
vessel B2 is empty of solids.
5.6.2 The height of overflow tube is adjusted to 15 cm (maximum) starting from
below the extraction vessel (or to the desired level).
5.6.3 Charge fresh solid in the extraction vessel (Section 5.4). Record the solid’s
weight.
5.6.4 Close valve V2, V5 and open valve V12. When the solvent starts to enter
the extraction vessel, immediately start the timer.

11
 5.6.5 Allow the solvent to fill the vessel until all solids are fully immersed in the
solvent. Keep on monitoring the solvent flow rate at FI-301. Record the
average flow rate value.
5.6.6 Close valve V12 to prevent more solvent from entering the extraction vessel
B2. Stop the timer and record the filing time to determine the volume of
solvent in vessel B2.
5.6.7 Reset and restart the timer. Let the extraction process take place for 10
minutes. In the meantime, make sure that vessel B3 is empty by opening
valve V10 and draining all liquid. Close back valve V10.
5.6.8 Temporarily switch off the heater W1 power to avoid flooding in the column.
5.6.9 Refill the reboiler with solvent if necessary.
5.6.10 After 10 minutes, collect 50 mL sample of the effluent for density
measurement by opening valve V5 and V3.
5.6.11 Continue the experiment for another 20 minutes.
5.6.12 Collect a 50 mL sample of the effluent for density measurement by opening
valve V5 and V3 after another 20 minutes.
5.6.13 Collect and measure all the effluent volume via valve V5 and V3.
5.6.14 Repeat the experiment with a fresh solid charge of the same weight and hot
solvent feed. Switch on the preheater W3 and adjust the temperature
controller TIC-103 set point to 50oC.

5.7 General Shut-Down Procedures

5.7.1 Open all vent valves V6, V7, and V9.
5.7.2 Place a container under valve V10. Open valves V4, V5 V8 and V10 to drain
all liquid from the equipment.
5.7.3 Shut-down the reboiler as follows:
a) Let the cooling water run. Switch off the heater W1.
b) Close the valve V12 for total reflux.
c) Allow the solvent in the reboiler to cool down to room temperature.
d) Empty the reboiler B1 by draining all liquid through valve V1.
5.7.4 Shut-down the cooling water flows as follows:
a) Let the cooling water run until the solvent in the reboiler has cooled down
to room temperature.
b) Close valve V13.
5.7.5 Clean the extraction vessel B2 as follows:
a) Ensure that the vessel B2 is drained of solvent.
b) Carefully remove the vessel cover and the solids container.
c) Discard the used solid and clean the container.
d) Carefully place the container back into the extraction vessel.
e) Replace the extraction vessel cover.
Note: Always clean the solids container thoroughly, especially the porous support,
to prevent molds from growing among the pores.
6.0 RESULTS
6.1 Sketch the process flow diagram for this experiment.
6.2 Record the data by using the table in Appendix 2.1 and 2.2.
6.3 Plot the calibration curve for solute composition.
6.4 Plot a graph to show the amount of solute extracted for every batch of experiment.
6.5 Estimate the extraction efficiency.

7.0 DISCUSSIONS
7.1 Discuss the finding of the graphs and results.
7.2 Evaluate the mass balance theory for this separation process.
7.3 Discuss any discrepancies and sources of error.

12
8.0 CONCLUSION
Based on the experimental procedure done and the results obtained, draw some
conclusions to this experiment.

13
 EXPERIMENT 3
YIELD AND EFFICIENCY DETERMINATION FOR CRYSTALLIZATION PROCESS

1.0 OBJECTIVE
1.1 To understand the crystallizer working principle.
1.2 To demonstrate the batch crystallization process utilizing the evaporative method.
1.3 To calculate and analyze the separation efficiency.

2.0 INTRODUCTION
Crystallization is a separation process where solid particles form within a
homogeneous liquid phase due to super-saturation induced either through cooling or
evaporation. The SOLTEQ Crystallizer (Model: BP123) has been designed to demonstrate
the basic principles of crystallization and the operation of a crystallizer equipment. The unit
consists of mainly a crystallizer vessel, crystallizer pump, feed/reaction vessel, dosing
pump, heat exchanger, condenser, product vessels and heating/cooling thermostats.
Appropriate devices and instrumentations are provided with the unit for controlling and
monitoring the process parameters.

3.0 THEORY
This SOLTEQ Crystallizer (Model: BP123) utilizes both the evaporation and cooling
methods for crystallization. In evaporation mode, liquid is removed from a saturated feed
solution to form super-saturation to allow the formation of crystals. Similarly, in the cooling
mode, the solution temperature is lowered to allow super-saturation. Various types of salt
solutions such as sodium chloride (NaCl), potassium chloride (KCl) and potassium nitrate
(KNO3) can be used to demonstrate different crystallization patterns, solubility behaviors
and phase formations. Furthermore, the cooling method enables different types of
products to be separated from a saturated solution in a solid form.

In the cooling method, the saturated solution is simply fed into the jacketed feed
vessel while the cooling thermostat set at the desired temperature. Crystals that form in
the vessel will accumulate at the bottom and can be drained out into a collection bottle.
On the other hand, for the evaporation method, a saturated solution is initially pre-heated
in a jacketed feed vessel before being fed into a circulation stream. The circulation stream
passes through a heat exchanger, where some of the water in the solution will evaporate.
The evaporated water vapor is then separated from the slurry in a crystallizer vessel and
emerges as condensate. The slurry is returned into the continuous circulation stream
through a propeller stirrer pump. The solid crystals that form in the circulation stream will
precipitate at the bottom and be collected in a product vessel.

4.0 MATERIALS AND EQUIPMENT

4.1 SOLTEQ crystallizer unit (Model: BP123)
SOLTEQ Crystallizer unit (Model: BP123) is a teaching unit comprising of several
components, as shown in Table 4.1. All glass components of the unit are made of
borosilicate 3.3 glass with PTFE gaskets. The equipment is also equipped with
temperature, flow and pressure control.

4.2 Safety Considerations

4.2.1 The unit must be operated under the supervisor of an authorized staff who
has been properly trained to handle the unit.
4.2.2 All operating instructions supplied with the unit must be carefully read and
understood before attempting to operate the unit.
4.2.3 Feed stock which severely affects PTFE, PFA and borosilicate glass are not
to be used.
4.2.4 The system should not be subjected to shock, sudden impact, vibration,
additional load, or permanent external action of aggressive vapors.

14
4.2.5 Always check and rectify any leak.
4.2.6 Do not touch the hot components of the unit.
4.2.7 Be extremely careful when handling hazardous, flammable or polluting
materials.
4.2.8 Restore the system to operating conditions after any repair job.
4.2.9 Make sure the system is sufficiently ventilated when working at atmospheric
pressure.
4.2.10 Do not exceed the maximum cooling water pressure of 2 bar (g) for the glass
coiled heat exchanger or condenser.
4.2.11 Only properly trained staff shall be allowed to carry out any servicing.
4.2.12 Before any servicing, shut down the whole operation and let the system to
cool down and be properly ventilated.
4.2.13 Do not use any coarse or abrasive cleaners on glass components.
4.2.14 Leaking couplings should be carefully retightened. Replace any gaskets or
seals if necessary.

Table 4.1. Detail description for each component in crystallizer unit.

No. Component Description
5 L jacketed cylindrical vessel made of
Feed/reaction borosilicate glass with stirrer and bottom outlet.
1
vessel (R1) Connected to a 0.2 m2 condenser to prevent
evaporation losses.
Measuring 0.5 L jacketed cylindrical vessel with graduations
2
vessel (B3) and made of borosilicate glass.
Dosing pump Longer peristaltic pump capable of handling solid
3
(P1) slurries, with up to 68.4 L/hr capacity.
Crystallizer DN150 cylindrical vessel made of borosilicate
4
vessel (B1) glass, having ports for vapor and liquid outlets.
Chemical resistant diaphragm vacuum pump
Vacuum pump
5 capable of ultimate pressure down to 4 mbar
(P2)
(abs) and maximum flow rate of 2.4 m3/hr.
Heat exchanger Steel tube heat exchanger to supply heat for
6
(W1) liquid evaporation, having 0.1 m2 exchange area.
Condensers High efficiency condensers made of stainless
7
(W2 & W3) steel with 0.432 m2 and 0.03 m2 exchange area.
1.5 kW external circulation thermostat bath with
Heating heating and temperature control. Filled with
8
thermostat (T1) thermal oil, operating temperature range between
ambient to 150oC.
2.0 kW external circulation thermostat bath with
Heating and both heating & cooling functions and temperature
9 cooling control. Filled with glycol-water solutions,
thermostat (T2) operating temperature range between -50oC to
100oC.
Product vessel 400 mL cylindrical vessel made of borosilicate
10
(B2) glass.
Condensate 400 mL cylindrical vessel with graduations and
11
vessel (B4) made of borosilicate glass.
Instruments and 6 temperature measurement points (TT101 –
12
Controls TT106).

15
 1 flow rate measuring point (FT-301).
1 pressure indicator (PT-201).

4.3 List of Materials

(i) Potassium chloride (KCl)
(ii) Sodium chloride (NaCl)
(iii) Potassium nitrate (KNO3)
(iv) Distilled water

4.4 List of Apparatus

(i) Balance
(ii) Measuring cylinders
(iii) Beakers
(iv) Hot plate
(v) Filter paper
(vi) Filter funnel
(vii)Oven

5.0 PROCEDURES
5.1 General Operating Procedures
5.1.1 Cooling water system – Cooling water is used as the cooling media. Hose
connections are such that the cooling water enters both condensers W2 and
W3 in parallel. Adjust each cooling water flow rates using valves V12 and
V13 to maximize cooling and condensation.
5.1.2 Heating thermostat (T1) – The heating thermostat’s temperature and pump
flow rate can be adjusted on the controller located on top of the thermostat.
Use the ‘up’ or ‘down’ button to change the temperature set point.
5.1.3 Heating/cooling thermostat (T2) – The heating/cooling thermostat’s
temperature can be adjusted on the controller located on top of the
thermostat. Press ‘SET’ and use the directional buttons on the controller to
adjust the temperature set point. If cooling is required, switch on the cooler.
Note: Do not switch on the cooler if the liquid temperature in the thermostat is more
than 30°C to avoid overloading the compressor.
5.1.4 Dosing pump (P1) - The feed flow rate of the pump can be controlled by
tuning the control knob on the pump itself.
Note: Do not operate the dosing pump P1 with valve W2 and W4 closed.
5.1.5 Vacuum pressure control (P2) – The vacuum pressure can be controlled by
adjusting the pressure set point of PIC-201 on the control panel. Press the
‘enter’ button once and use the ‘up’ or ‘down’ button to change the pressure
set point.
5.1.6 Stirrer drive (M1) – Turn the speed control knob on top of the stirrer drive to
adjust the stirrer’s speed.

5.2 General Start-Up Procedures

5.2.1 Ensure all valves are closed except the ventilation valve V16.
5.2.2 Check that the product vessel B2 is empty of liquid and properly connected
to valve V5 at the circulation line.
5.2.3 Prepare the 1.5L of feed solution containing the desired substances to be
crystallized. Pour the solution into the 10 L feed/reaction vessel R1 through
the charge port by opening valve V7. Heat and stir the supersaturated
solution at high temperature but below the boiling point of water.
Note: The feed solution should preferably be saturated to minimize the time taken
for crystallization to occur. Calculate the amounts by using the solubility curve:
Appendix A6.

16
 5.2.4 Switch on the stirrer M1 and adjust the speed to mid-range.
5.2.5 Ensure that the cooler T2 contains sufficient heat transfer fluid (glycol-water
solution). Refill as necessary.
5.2.6 Turn on the cooling water flow by opening valves V12 and V14.
5.2.7 For cooling crystallization, the unit is now ready for experiments.
5.2.8 For evaporative crystallization, open valve V9, V10 and V16. Open valve
V8 and fill in the feed solution through the charge port of crystallization
vessel, B1.
5.2.9 Switch on heater T1. Set the temperature of thermostat T1 to 150oC.
5.2.10 Open valve V4. Then, switch on the peristaltic pump P2 and set the
circulation flow rate to 1 LPM. Observe the liquid solution flowing from the
crystallizer vessel B1 through the pump to the heat exchanger W1 and then
overflowing at the conical inlet back to the crystallizer vessel.

5.3 Sample / Product Collection (For evaporative crystallization only)

5.3.1 Use 100 mL beaker for sample collection or 2 L vessel for product collection.
Make sure that the product vessel B2 is empty.
5.3.2 Fully open valve V5 and let the slurry solution flow from the circulation line
into the product vessel.
5.3.3 Collect the required amount of slurry in vessel B2 and close valve V5 and
V6.
5.3.4 From the beaker, pour the slurry solution through a filter to obtain the
crystallized solid. Dry the solid in an oven (100°C).

5.4 Draining of Condensate

Open valve V11 to drain the condensate vessel B4.

5.5 Experimental Procedures

(A) Batch Cooling Crystallization
5.5.A.1 Perform general start-up procedures to step 7 as described in Section 5.2.
5.5.A.2 Switch on thermostat T2 and set the cooling temperature to -20°C. Start the
timer.
5.5.A.3 Observe the temperature drop in the feed/reaction vessel R1 until it has
reached a constant value. Record the temperature value at every 30 minutes
intervals.
5.5.A.4 Observe the formation of crystals in vessel B1. If crystals start to appear, let
the process run for another 5 minutes.
5.5.A.5 After 5 minutes, stop the timer and switch off the stirrer M1. Allow the newly
formed crystals to settle to the bottom of the feed/reaction vessel R1.
5.5.A.6 Open valve 1 to fill the measuring vessel B3 with 400ml of solution containing
crystals from vessel R1. Close valve V1.
5.5.A.7 Immediately place a beaker below valve V2 and open valves V2 and V3 to
collect the product slurry solution.
5.5.A.8 From the beaker, quickly pour the slurry solution through a filter to obtain the
crystallized solid. Dry the solid in an oven and measure the weight of solid
collected.

(B) Batch Evaporative Crystallization

5.5.B.1 Perform general start-up procedures to step 10 as described in Section 5.2.
5.5.B.2 Set the circulation flow rate to 1 LPM and the temperature of thermostat T1
to 150oC, Make sure that the feed solution will boil at the specified
temperature and pressure.
5.5.B.3 Allow the circulation line to heat up until boiling and evaporation occurs, and
condensate starts to appear in the condensate vessel B4. Start the timer.

17
 5.5.B.4 Record the circulation flowrate (FT301) and inlet/outlet temperatures (TT101
- 104) of both feed solution and thermal fluid through the heat exchanger
W1.
5.5.B.5 Observe the formation of crystals in the circulation line. Once crystals start
to appear, stop the timer and record the time duration. Restart the timer.
Note: Formation of crystals may take some time, especially if the feed solution is
not saturated.
5.5.B.6 Measure the amount of condensate accumulated in vessel B4 and drain the
condensate vessel according to Section 5.4.
5.5.B.7 Perform the following steps at every 30 minutes:
(a) Record the circulation flowrate and inlet/outlet temperatures of both
slurry solution and thermal fluid through the heat exchanger W1.
(b) Collect 100 mL samples as explained in Section 5.3.
(c) Determine the amount of crystals obtained and the crystal concentration
in the crystallizer.
(d) Measure the amount of condensate accumulated in vessel B4.
(e) Drain the condensate vessel B4 according to Section 5.4.
5.5.B.8 Carry out step 7 until the liquid level in the crystallizer B1 has dropped to
about halfway below the conical inlet. It should take between 1-2 hours.
5.5.B.9 Record the total time taken for the crystallization process.
5.5.B.10 Collect 500 mL of product slurry from the circulation line as explained in
Section 5.3.
5.5.B.11 Determine the amount of crystals obtained and the crystal concentration in
the crystallizer at the end of the experiment.

5.6 General Shut-Down Procedures

5.6.1 Keep the cooling water running through condensers W2 and W3.
5.6.2 Switch off thermostats T1 & T2, stirrer M1, and dosing pump P1.
5.6.3 Switch off vacuum pump P2 and release the vacuum by opening valve V16.
5.6.4 If the evaporative crystallization process was carried out, set the dosing flow
rate of pump P1 to 1 LPM and allow the liquid cool down to less than 50oC
before turning off the dosing pump P1.
5.6.5 Close valve V12 and V14 to stop the cooling water flow.
5.6.6 Open valve V5 to drain all liquid from the circulation line.
5.6.7 To clean the solid residue in the circulation line, open V9 and V13, but close
V10, V12, and V14 to allow water flushes to B1 and some to B4. Drain the
water through valves V2, V5, V6 and V11.
5.6.8 If required, drain the liquid in the feed/reaction vessel R1 by opening valves
V1, V2 and V3.
5.6.9 To clean the solid residues in vessel R1, open V7 and pass a hose through
the charge port and flush the vessel with tap water. Drain the water through
valve V2 and V3.
5.6.10 Close all the remaining valves.

6.0 RESULTS
6.1 Record the data by using the table in Appendix 3.
6.2 For (A): Plot the graph of crystal composition against time and mark the time when
crystals begin to appear.
For (B): Plot the graph of crystal composition in the circulation line against time.
6.3 For (A): Determine the amount of crystals obtained.
For (B): Determine the condensate flow rate, product slurry flow rate and amount of
crystals obtained.
For both, perform material balance on the crystallizer and calculate the
crystallization yield (refer Appendix A5-A7).
6.4 Determine the heat transferred to / from the circulation line. For (B), calculate the

18
 heat of evaporation as well. Then, perform energy balance on the crystallizer and
calculate the heat of crystallization (refer Appendix A5-A7).
7.0 DISCUSSIONS
7.1 Sketch the process flow diagram for this experiment.
7.2 Discuss the finding of the graphs and results.
7.3 Evaluate the mass balance theory for this separation process.
7.4 Discuss any discrepancies and sources of error that influence the reproducibility of
the experimental result.

8.0 CONCLUSION
Based on the experimental procedure done and the results obtained, draw some
conclusions to this experiment.

19
 EXPERIMENT 4
YIELD AND EFFICIENCY DETERMINATION FOR CENTRIFUGATION PROCESS

1.0 OBJECTIVE
1.1 To understand the centrifuge working principle.
1.2 To demonstrate the batch centrifugation of a homogeneous lipid-water solution.
1.3 To analyze and differentiate the separation efficiency of the said solution.

2.0 INTRODUCTION
Centrifugation process exploits the effect of differential centrifugal force acting
on the particles of a solution. As the main driving force, centrifugal force can be applied
on the fluid of interest to move the particles away from the axis of rotation. Though all
particles would eventually move further away from the axis of rotation, these particles,
different in density, would experience different magnitude of centrifugal force, thus
affecting their extend of movement within the fluid. As such, the separation of denser
particles from the fluid could be achieved.

The SOLTEQ Disc Bowl Centrifuge (Model: FD15) has been designed to
demonstrate the basic principles of centrifugation of a homogeneous solution. In this
experiment, it is to provide practical training in the technique of separating a heavy phase
liquid from a lighter phase liquid with particular emphasis on the separation of cream from
milk. The unit applies the centrifugal force to the fluid using its rotating discs. The denser
particles (skimmed milk) move further away from the axis of rotation while the lighter
substance (fats) exits near the center. Thus, the cream and skimmed milk will be obtained
as the product.

3.0 THEORY
Centrifugation is a separation process used in the food industry for the treatment
of milk, principally for the standardization of milk and milk product, and in the production
of cream or skim milk. This process uses centrifugal force to separate two mixed liquids or
insoluble solids from liquids. The disc centrifuge is equipment which works like a normal
centrifuge but with continuous supply of fluid feed and continuous fluid output. This
equipment applies centrifugal force to the fluid feed using rotating disc. The denser
particles move further away from the axis of rotation while the lighter substance exits near
the center. Such working principle of disc bowl centrifuge is illustrated in Figure 5.1.

Figure 5.1: A typical working principle of a disc bowl centrifuge unit.

20
4.0 MATERIALS AND EQUIPMENT
4.1 SOLTEQ Disc Bowl Centrifuge unit (Model: FD15)
The specification and the part description of the SOLTEQ Disc Bowl Centrifuge unit
(Model: FD15) is shown in Table 5.1 and Figure 5.2, respectively.

Table 5.1. Specification of the Disc Bowl Centrifuge

Capacity : 125 – 130 Litres / hour
Motor Power : 70W
Maximum rotating speed : 9500 rpm
: 21 (11 relief disc; 10 plain
Number of discs
disc)
Milk container : Stainless steel
Float chamber material : Stainless steel
Body material : Durable plastic
Max container capacity : 12L

Figure 5.2: Solid-liquid extraction unit.

4.2 Safety Considerations

4.2.1 All parts of the top bowl should be cleaned with hot water in which you should
add some detergent.
4.2.2 Rest of milk, cream or other impairs should be cleaned with soft duster or
cleaning brush. Specially take care to clean very precisely all the holes in
the top bowl upper part, top bowl bottom part and in adjusting screw. For
cleaning this parts, cleaning brush is recommended. Other parts of the
separator that come in contact with milk, should also be cleaned with hot
water in which some detergent is added. Then, rinse parts in clean water.
4.2.3 If milk or cream rests get dry, do not remove them with sharp objects or
sharp duster. It can ruin galvanic protection cover or plastic parts.
4.2.4 Before cleaning cream separator housing, make sure to disconnect the
power supply. Clean the housing with wet duster, followed by the dry duster.
4.2.5 Device is protected against direct water access, but care should be taken to
avoid that water comes into the device.

21
 4.2 List of Materials
(i) Full cream milk
(ii) Low fat high calcium milk
(iii) Fresh Milk

4.3 List of Apparatus

(i) Measuring cylinders
(ii) Beakers
(iii) Weighting balance

5.0 PROCEDURES
5.1 General Start-Up Procedures
5.1.1 Make sure the milk sample is around 30 – 35 °C. You cannot skim milk with
temperature lower than 30 °C
5.1.2 Switch on the disc bowl centrifuge with switch 0/1 and wait for 30 seconds
until the top bowl reaches working speed.
Note: The unit comes with a signal lamp. By switching on disc bowl centrifuge, the
indicator will shine red and when the unit reaches working speed, it will start to shine
green.
5.1.3 Make sure the closing cork is initially in close position.
5.1.4 When the indicator shines green, the centrifuge is ready for experiment.

5.2 Experimental Procedures

5.2.1 Double check the centrifuge indicator (green).
5.2.2 Double confirm that the closing cork is initially in close position.
5.2.3 Place 1 liter beaker below the skimmed milk funnel and 400 ml beaker below
the cream funnel.
5.2.4 Pour 1 liter of the full cream milk into the top milk container.
5.2.5 Turn the closing cork to open position. The end of the closing cork is turned
to the cut in the container and the flow is opened.
5.2.6 The skimmed milk will start to flow out from the skimmed milk tunnel, follow
by the cream at cream funnel.
5.2.7 Wait until all the skimmed milk and cream is completely separated.
5.2.8 Measure the volume of obtained skimmed milk and cream with measuring
cylinder.
5.2.9 Repeat the procedure with low fat milk (or different brand). Make sure to
clean and dry the parts before repeating the experiment.

5.3 General Shut-Down Procedures

5.6.1 Turn off the switcher 0/1 and wait until the top bowl reached stationary state.
5.6.2 Dismantle the milk container, floating device, holder for milk container and
top bowl.
5.6.3 Clean all the dismantled components.
5.6.4 To clean the top bowl, unscrew the top bowl fixing nut.
5.6.5 Separate all different pieces (plastic partition, metal discs and rubber
washer) and clear them with hot water. To achieve better results, cleaning
detergents can be added to the hot water.
5.6.6 Dry all the components.

6.0 RESULTS
6.1 Record the data by using the table in Appendix 4.
6.2 Determine the percentage of cream in each of the milk used in the experiment using
both mass and volume data.

22
7.0 DISCUSSIONS
7.1 Discuss the finding of the results.
7.2 Explain the separation principle of full cream milk using disc bowl centrifuge unit.
7.3 Write the mass balance equations for this separation process, using cream (fat) and
skimmed milk as the only compounds in the solution.
7.3 Compare the advantages and disadvantages of this centrifuge system.
7.4 Discuss any discrepancies and sources of error that influence the reproducibility of
the experimental result.

8.0 CONCLUSION
Based on the experimental procedure done and the results obtained, draw some
conclusions to this experiment.

23
 EXPERIMENT 5
YIELD AND EFFICIENCY DETERMINATION FOR MEMBRANE SEPARATION PROCESS

1.0 OBJECTIVES
1.1 To demonstrate the reserve osmosis via membrane separation technology.
1.2 To evaluate the efficiency of membrane separation process based on reverse
osmosis system.

2.0 INTRODUCTION
Membrane filtration is a technology that undertakes physical separation process
using pressure. It provides effective separation without the use of heating energy as in
distillation processes. Reverse osmosis (RO) is a filtration method that removes many
types of large molecules and ions from liquid by applying pressure to the solution when it
is one side of a selective membrane. The result is that the solute is retained on the
pressurized side of the membrane and the pure solvent is allowed to pass to the other
side.

3.0 THEORY
In osmosis, a spontaneous transport of solvent occurs from a dilute solute or salt
solution to a concentrated solute or salt solution across a semipermeable membrane which
allows passage of the solvent but impedes passage of the salt solutes. In Figure 6.1, the
water (solvent) flows through the semipermeable membrane to the salt solution. The levels
of both liquids are the same. The solvent flow can be reduced by exerting a pressure on
the salt-solution side and membrane (Figure 6.1b). At a certain pressure called the osmotic
pressure, π of the salt solution, equilibrium is reached and the amount of the solvent
passing in the opposite directions are equal. The chemical potentials of the solvent on both
sides of the membrane are also equal. The properties of the solution is determined only
by the value of the osmotic pressure, not the membrane, provided that it is truly
semipermeable. To reverse the flow of the water so that it flows from the salt solution to
the fresh solvent (Figure 6.1c), the pressure is increased above the osmotic pressure on
the solution side.

Figure 6.1. Osmosis and reverse osmosis phenomenon: (a) osmosis, (b) osmotic
equilibrium, and (c) reverse osmosis.

This phenomenon is called reverse osmosis, which is used in a number of

processes. An important commercial use is in the desalination of seawater or brackish
water to produce fresh water. Unlike distillation and freezing processes, to remove
solvents, reverse osmosis can operate at ambient temperature without any phase change.
This process is especially useful for the processing of thermally and chemically unstable
products. Applications include concentration of fruit juices and milk, recovery of protein
and sugar from cheese whey, and the concentration of enzymes.

4.0 MATERIALS AND EQUIPMENTS

4.1 SOLTEQ Membrane Filtration Unit (Model: TR16)
The SOLTEQ Membrane Filtration Unit (Model: TR16) is supplied with Polyamide Film

24
(AFC99) for reserve osmosis, Polyamide Film (AFC30) for the nanofiltration, and PVDF
membrane (FP200) for the ultrafiltration operations, as shown in Figure 6.2. Table 6.1
and 6.2 shows the description for all the components and control valves installed in
the membrane filtration unit, respectively.

Figure 6.2. Membrane filtration unit.

Table 6.1. Description for all components installed in the membrane filtration unit.
No. Component
1 Triple Plunger Pump (P1)
2 Centrifugal Pump (P2)
3 Feed Tank
4 Product Tank
5 Heating/Cooling Tank
6 Plate Heat Exchanger
7 Flowmeter (FT1)
Differential Pressure
8 Range: 0 – 5000mm H20
Transmitter (DPT1)
9 Pressure Transmitter
Description
The triple plunger pump is used to pump
the liquid from the feed tank into the
membrane module. A Pressure regulator is
installed to regulate the operating pressure
of the feed system.
The centrifugal pump is used to circulate
the liquid from the plate heat exchanger to
the water tank.
Capacity: 15 L; Material: Stainless Steel
316
Capacity: 15 L; Material: Stainless Steel
316
Capacity: 50 L; Heater: 11.5kW; Coil
Surface Area: 0.2 m2
Heat Exchange Area: 0.26 m2; Design
Pressure: 10.0 bar; Design Temp: 100°C;
Wetted Material: Stainless Steel 316
Range: 0 – 20 LPM
Range: 0 – 100 bar

25
 (PT1)
Temperature Transmitter
10 Range: 0 – 100°C
(TT1 – TT5)
Pressure Gauge (PI1 –
11 Range: 0 – 70 bar
PI3)
12 Temperature Gauge (TI1) Range: 0 – 100°C
Table 6.2. Description for all control valves installed in the membrane filtration unit.
Item Description Type
V1 Product tank drainage valve. 2-way
V2 Product tank outlet flow into the plunger pump/feed tank 2-way
for sample reuse
V3 Feed tank outlet flow into the plunger pump 2-way
V4 Feed tank drainage valve 2-way
V5 Flow shut off for operating pressure setting 2-way
V6 Drainage valve 2-way
V7 Controls of the retentate flow rate and to vary ΔP Needle
V8 Retentate sampling valve 2-way
V9 Permeate sampling valve 2-way
V10 Hot water tank drainage valve 2-way
V11 Control of the cooling media out flow rate Globe
V12 Water supply to the heating/cooling tank 2-way
V13 Control of the flow rate of water fed back from heat Globe
exchanger to vary the temperature of the system

4.3 List of Materials

(i) Potassium chloride (KCl)
(ii) Distilled water

4.4 List of Apparatus

(i) Balance
(ii) Measuring cylinders
(iii) Beakers
(iv) Digital conductivity meter

5.0 PROCEDURES
5.1 General Operating Procedure
5.1.1 Pumps and Pressures
a) In order to set the maximum working pressure, close valve V5.
b) Use a wrench to adjust the pressure regulator to a safe low pressure
setting by turning the pressure adjuster nut in counter-clockwise.
c) Be sure that the feed tank is not empty. Open valve V3 and close valve
V2, then switch on the plunger pump P1. Observe the pressure gauge
PI1 reading next to the pressure regulator. The pressure will rise steadily
until it reaches the previously set pressure.
d) Using a wrench, adjust the pressure regulator to obtain the desired
maximum working pressure (clockwise to increase pressure; counter-
clockwise to decrease pressure).
e) Re-open the valve V5 for the liquid to flow.
Note: If the pressure fails to increase or keeps dropping, there must be air trapped
in the membrane system. Shut off the pump and let the air to escape. Make sure no
air being introduced into the system.

26
 5.1.2 Heat Exchanger
The TR16 is equipped with a plate heat exchanger which is connected to a
heating/cooling tank. Before operating the plate heat exchanger, please
ensure that the liquid level inside the tank is always above the heater
element. Set the desired temperature at temperature controller on the
control panel. Subsequently, switch on the centrifugal pump P2 to circulate
the liquid through the heat exchanger. Use globe valve V13 to vary the water
flow rate.
Note: Plunger pump generates heat during the operation, circulate cooling water or
refrigerated medium to achieve the required temperature if necessary.

5.1.3 Draining the Leftover

Before flushing the membrane, the leftover liquid has to be completely
drained after each session in order to prevent bacterial formation overnight.
There are six drainage points with the TR16 unit. For a complete drainage
of the system (excluding the heating tank), open all valves except valve V10.

5.2 Before Operation

5.2.1 Perform a quick inspection to ensure that the unit is in proper operating
condition.
5.2.2 Connect the unit to the nearest power supply.
5.2.3 Prepare the accessories/chemical needed for the experiment, such as hand-
held digital conductivity meter and probe is working properly, and sodium
chloride (salt).

5.3 Experimental Procedure (Reverse Osmosis: Salt Rejection from Water)

5.3.1 Insert 2 RO membranes (AFC99) into the membrane module. Secure the
rubber seal well on both ends of the membrane, make sure it doesn’t fold.
Tighten the screw and make sure no leakage.
5.3.2 Prepare 10L salt (NaCl) solution with a concentration of 2 g/L.
5.3.3 Set the maximum working pressure at 35 bars.
5.3.4 Make sure that all valves are set as follows:
Open Close Leave Alone
V1, V2, V4, V6, V8,
V3, V5, V7 V11, V13
V9, V10, V12
5.3.5 Fill up the feed tank with the salt water prepared in step 2. Switch on the
centrifugal pump P2 to circulate the cold water through the plate heat
exchanger.
5.3.6 Open the main water supply to flow in water through the cooling coil. Adjust
the globe valve V13 and V11 until desired working temperature is achieved
and stabilized before taking the result.
5.3.7 Start the plunger pump. Set inlet pressure to 10 bars by adjusting the needle
valve V7 and let the water flow for about 1 minute until the flow rate is stable
before taking any reading.
5.3.8 While the plunger pump running, open the bleed screws on both HI and LO
side of the differential pressure transmitter slowly to bleed the air trapped
inside the system. (if this is not done, the differential pressure reading will
be unstable)
5.3.9 Open the sampling valve V9 and drain-off the water leftovers from the last
experiment. Record the volume of the collected permeates every 1 minute
for at least 15 minutes. Measure the increase in conductivity in the feed tank.
5.3.10 Stop the plunger pump and close valve V3. Mix all the filtrate and retentate
back into the feed tank by opening valve V12, then stir the mixture.

27
 5.3.11 Repeat the experiment (step 5 to 10) at this time vary the inlet pressure by
a factor of 5 bars up to 25 bars by manipulating the needle valve V7.

6.0 RESULTS
6.1 Sketch the process flow diagram for this experiment.
6.2 Record the data by using the table in Appendix 5.
6.3 Plot graph of salt conductivity in the feed tank versus time at different ∆P.
6.4 Estimate the separation efficiency for different ∆P.

7.0 DISCUSSION
7.1 Discuss the finding of the graphs and results.
7.2 Compare the membrane performance based on different pressure drop.
7.3 Evaluate the error and precaution steps needed in this experiment.
7.4 Suggest a suitable method for cleaning membrane used in this experiment.

8.0 CONCLUSION
Based on the experimental procedure done and the results obtained, draw some
conclusions to this experiment.

28
 EXPERIMENT 6
EFFECT OF REGULATING REFLUX RATIO ON TOP PRODUCT COMPOSITION IN
DISTILLATION PROCESS

1.0 OBJECTIVES
1.1 To perform batch distillation on a binary mixture using a continuous distillation
column and regulate the reflux ratio.
1.2 To study the effect of regulating reflux ratio on the purity of the top product.

2.0 INTRODUCTION
Distillation process is widely applied in the engineering industry for mass transfer
and separation operations. This is done by vaporization of a liquid mixture of miscible and
volatile substances into individual components.

3.0 THEORY
3.1 Overview
Distillation is simply defined as a process in which a liquid or vapor mixture
of two or more substances is separated into its component fractions of desired purity,
by the application and removal of heat. The process is based on the fact that the
vapor of a boiling mixture will be richer in the components that have lower boiling
points. Hence, when this vapor is cooled and condensed, the condensate will contain
more volatile components. At the same time, the original mixture will contain more of
the less volatile material.

The primary equipment employed in the process of distillation are distillation

columns, which are designed to achieve this separation efficiently. Although the
layman has a fair idea as to what “distillation” means, the important aspects that
seem to be missed from the manufacturing point of view are: (1) distillation is the
most common separation technique; (2) it consumes enormous amounts of energy,
both in terms of cooling and heating requirements; (3) it can contribute to more than
50% of plant operating costs. The best way to reduce operating costs of existing
units is to improve their efficiency and operation via process optimization and control.
To achieve this improvement, a thorough understanding of distillation principles and
how distillation systems are designed is essential.

As stated, distillation is the process of heating a liquid until some of its

ingredients pass into the vapor phase, and then cooling the vapor to recover it in
liquid form by condensation. The main purpose of distillation is to separate a mixture
by taking advantage of different substances’ readiness to become a vapor. If the
difference in boiling points between two substances is great, complete separation
may be easily accomplished by a single-stage distillation. If the boiling points differ
only slightly, many re-distillations may be required. In the simplest mixture of two
mutually soluble liquids with similar chemical structures, the readiness to vaporize of
each is undisturbed by the presence of the other. The boiling point of a 50-50 mixture,
for example, would be halfway between the boiling points of the pure substances,
and the degree of separation achieved by a single distillation would depend only on
each substance’s readiness to vaporize at this temperature. This simple law was first
stated by 19th- century by the French chemist Frangois Marie Raoult (known
as Raoult ’s law).

3.2 Vapor-Liquid Equilibrium Relationship

Since the boiling point properties of the components in the mixture being
separated are so critical to the distillation process, the vapor-liquid equilibrium (VLE)
relationship is of importance. Specifically, it is the VLE data for a mixture which
establishes the required height of a column for a desired degree of separation.

29
Constant pressure VLE data is derived from boiling point diagrams, from which a
VLE curve can be constructed; like the one illustrated in Figure 7.1 for a binary
mixture. The VLE plot shown expresses the bubble-point and the dew-point of a
binary mixture at constant pressure. The curve is called the equilibrium line, and it
describes the compositions of the liquid and vapor in equilibrium at a constant
pressure condition.

Figure 7.1. VLE plot showing equilibrium

curve.

Figure 7.1 shows the VLE plot for a binary mixture that has essentially a
uniform equilibrium, and therefore represents a relatively easy separation. However,
there are many cases where non-ideal separations are encountered. These more
difficult distillations are defined by the examples shown in Figure 7.2. An important
system in distillation is an azeotropic mixture. An azeotrope is a liquid mixture which
when vaporized, produces the same composition as the liquid. The VLE plots
illustrated in Figure 7.3 shows two different azeotropic systems: one with a minimum
boiling point and one with a maximum boiling point. In both plots, the equilibrium
curves cross the diagonal lines.

Figure 7.2.
Examples of non-ideal
VLE curves.

30
 Figure 7.3. Examples
of VLE curves for
azeotropic systems.

The design of
a distillation column is based on information derived from the VLE diagram describing
the mixtures to be separated. The vapor-liquid equilibrium characteristics are indicated
by the characteristic shapes of the equilibrium curves. This is what determines the
number of stages, and hence the number of trays needed for a separation. Although
column designs are often proprietary, the classical method of McCabe-Thiele for binary
columns is instructive on the principles of design.

McCabe-Thiele is a graphical design that uses the VLE plot to determine the
theoretical number of stages required to effect the separation of a binary mixture. It
assumes constant molar overflow. This implies that the molal heats of vaporization of
the components are roughly the same. In addition, it is assumed that heat effects
(heats of solution, heat losses to and from column, etc.) are negligible, and that for
every mole of vapor condensed, 1 mole of liquid is vaporized. The design procedure
is as follows. Given the VLE diagram of the binary mixture, operating lines are drawn
first. The operating lines define the mass balance relationships between the liquid and
vapor phases in the column. There is one operating line for the bottom (stripping)
section of the column, and one for the top (rectification or enriching) section of the
column. Use of the constant molar overflow assumption also ensures that the operating
lines are straight lines. The operating line for the rectification section is constructed as
follows: First the desired top product composition is located on the VLE diagram, and
a vertical line produced until it intersects the diagonal line that splits the VLE plot in
half. A line with slope R/(R+1) is then drawn from this intersection point. Refer to Figure
7.4 for illustration of the procedure.

Figure 7.4. Application of MCCabe-Thiele to VLE diagram.

4.0 MATERIALS AND EQUIPMENT

31
4.1 Description of Apparatus
Figure 7.5 shows a sieve plate distillation column comprises of 8 plates. One of the
plates is clearly shown during the distillation process via the borosilicate glass
section. Sieve plates are designed to illustrate the actual plant column construction
with underflow weir and downcomer. A coil type overhead condenser made of
stainless steel is connected to the top of the column to condense the product vapors
to be collected at the reflux divider. Reflux control is made possible from 0 – 100%
via electronic control valves. A glass product collector sits below the reflux divider
with a sample port fitted for collection of final product to be analyzed. A stainless
steel fully insulated reboiler is connected at the base of the column to evaporate
process substances. A jet vacuum pump fitted at the top product line allows
vacuumed distillation operation.

Figure 7.5. Distillation column unit.

4.1 Technical Specifications

4.2.1 60 mm diameter sieve plate column made of stainless steel and borosilicate
glass containing 8 sieve plates with downcomers and underflow weirs; every
plate incorporates a temperature sensor positioned to accurately measure
the liquid temperature.
4.2.2 10 L electrical heated reboiler made of stainless steel with sight level glass
and full insulation; level switch and digital temperature controller included for
protection with low level warning alarm; comes with internal overflow during
continuous operation.
4.2.3 Overhead coil type condenser made of borosilicate glass to allow vapor and
condensate to be viewed, comes with cooling water flow meter.
4.2.4 Condensate collector made of borosilicate glass with double overflow weirs
and exit pipes to allow separation of immiscible liquids.
4.2.5 Reflux return valve, electrical operated to allow reflux setting of 0 – 100%
via signal.
4.2.6 Differential manometer connected to measure column top and bottom
pressure drop.
4.2.7 Jet pump for vacuum down to 200 mbar (abs); comes with pressure gauge.
4.2.8 2 x 10 L cylinder feed tanks made of stainless steel.
4.2.9 10 L cylindrical glass product tank with drain and venting port.

32
 4.2.10 Chemical resistant feed pump – 18 L/h.
4.2.11 Dosing feed vessel connected to the column for continuous addition of third
liquid component which together with the condensate phase separator
vessel, allows study of azeotropic distillation.
4.2.12 Bottom product heat exchanger which maybe water cooled or used as feed
pre-heater.
4.2.13 Maximum process temperature 130 oC.
4.2.14 Heater capacity 2000 W.
4.2.15 Heater power controller with transducer.
4.2.16 Water flow meter 0 – 400 L/j.
4.2.17 15 point thermocouple measurement with digital display.
4.2.18 Column pressure gauge.
5.0 PROCEDURES
5.1 Chemical Preparation (Distilled Water/Ethanol Mixture)
To prepare a mixture of composition (X%) of ethanol, observe the following steps:
5.1.1 Fill a 1 L measuring cylinder with X mL of ethanol.
5.1.2 Pour ethanol into a 1 L beaker.
5.1.3 Fill the beaker up to 1 L with distilled water.
5.1.4 Stir using a glass rod.
5.1.5 The product is now a 1 L batch binary mixture with X% (v/v) of component
A.
*As an example, to create a 35% (v/v) mixture of ethanol, pour 350 mL of ethanol into
a beaker, and fill the beaker up to 1 L with distilled water.
Note: Ethanol is volatile and will evaporate quickly. Avoid exposing this chemical to the
atmosphere for extended periods of time.

5.2 Refractive Index Graph Preparation

To obtain the refractive index data for ethanol-water solution:
5.2.1 Prepare 100 mL distilled water.
5.2.2 Prepare 10 mL of ethanol.
5.2.3 Measure the refractive index for both distilled water and ethanol by digital
handheld refractor meter.
5.2.4 Record the refractive index.
5.2.5 Dilute 10 mL of ethanol with 100 mL of distilled water in a beaker. Then
measure the refractive index by refractor meter.
5.2.6 Add another 10 mL of ethanol into beaker and measure the refractive index.
Repeat this procedure until 100 mL of ethanol is added.
5.2.7 Prepare 100 mL of ethanol and 10 mL of distilled water in a beaker. Measure
the refractive index by refractor meter.
5.2.8 Add another 10 mL of distilled water into the same beaker. Repeat the
procedure until 90 mL of distilled water is added.
5.2.9 Record down the pressure and temperature reading in Appendix 6.1.

5.3 Experimental Pre-Procedure

5.3.1 Place the distillation column on a floor level.
5.3.2 Plug the 3-pin plug to the 240 VAC main power supply. Turn ON the power
supply.
5.3.3 Switch ON the power supply unit on the control panel.
5.3.4 Connect cooling water inlet and outlet to the main water hose.
5.3.5 Shut down all valves.
5.3.6 Fill the evaporator tank with solution of ethanol-distilled water.
5.3.7 Open vacuum cooling inlet (V10) and vacuum valve (V9) to vacuum top
product condenser and reflux tank. Leave it for 10 minutes.
5.3.8 Close the vacuum valve (V9).
5.3.9 Open the cooling water inlet (V11).

33
 5.3.9 Close the vacuum cooling inlet (V10).

5.4 Experimental Procedure

5.4.1 Prepare a 10 L batch of binary mixture (Section 5.1) of known composition.
5.4.2 Collect a 10 mL sample using a syringe and determine the refractive index.
5.4.3 Record the refractive index as shown in Appendix 7.
5.4.4 Pour the mixture into the evaporator tank.
5.4.5 Setup the unit according to experiment pre-procedure (Section 5.3).
Note: Do not open the vacuum valve of V10 and V9 for the vacuum pump during
the experiment. Operation of the vacuum pump after the mixture is partially
vaporized will cause the fluids to gush upwards, damaging the column.
5.4.6 Set the temperature of the evaporator tank (T13) at 90oC using the
temperature controller.
5.4.7 Using the potentiometer, set the reflux to 100%.
5.4.8 Once the top product appears in the phase break vessel, run the column at
total reflux for another 10 minutes.
5.4.9 Record down all the temperatures in Appendix 6.2.
5.4.10 Take a sample from evaporator tank and phase break vessel and measure
the refractive index.
5.4.11 Using the potentiometer, set the reflux ratio to the between 50%.
5.4.12 At the intervals of 10 minutes, record down all temperatures and draw a
sample from the top product tank (T5) and evaporator tank (T2). Measure
and note down the refractive index of each sample. To quickly cool down the
evaporator sample, place the test tube in a beaker filled with ice water.
5.4.13 Increase the reflux by 20% after each interval until 90% reflux.
5.4.14 Take 3 readings each. Then, empty the top product vessel and measure its
volume.
5.4.15 Tabulate the data obtained in Appendix 6.3.
5.4.16 After the experiment, drain off the contents in the evaporator tank, phase
break vessel and top product tank. All samples can be re-used after the
experiment, as long as they are uncontaminated.
5.4.17 Switch off the main power switch and power supply. Turn off the water supply
and disconnect the hoses.

6.0 RESULT
6.1 Record the data by using the table in Appendix 6.1, 6.2, and 6.3.
6.2 Plot the graph of refractive index vs. mass fraction of ethanol.
6.3 Construct a T-x-y diagram.
6.4 Evaluate the q-line value.
6.5 Determine the theoretical stages required for this separation process.

Useful Data:
Heat capacity of ethanol = 158.8 kJ/kmol.oC.
Heat capacity of water = 75.4 kJ/kmol.oC.
Ethanol-water vapor liquid equilibrium data at 1 atm is given as Appendix A8.

7.0 DISCUSSION
7.1 Sketch the process flow diagram for this experiment.
7.2 Discuss the finding of the graphs and results.
7.2 Discuss the effect of regulating reflux ratio on the purity of the top product.
7.3 Compare the column performance based on different reflux ratio.

8.0 CONCLUSION
Based on the experimental procedure done and the results obtained, draw some
conclusions to this experiment.

34
Appendix 1
Feed Solvent Raffinate Extract
Solvent
Flow Flow Time Solute Solute
to Feed Refractive Refractive
Rate Rate (min) Composition Composition
Ratio Index Index
(L/min) (L/min) (wt%) (wt%)

Appendix 2.1: Calibration data for solute composition

Solute Composition Weight Volume
Mass of Mass of
(g oil / of of Density
Peanut ethanol (g oil /
g solution solution (g/mL)
Oil (g) (g) g solvent)
solution) (g) (mL)
0 100
20 100
40 100
60 100
80 100
100 100

Appendix 2.2
Mass of solids = ___________ kg
Solvent density = ______________ g/mL
Average solvent flow rate = _____________ mL/min
Solvent Effluent Amount Retained
Contact Solvent
Filling of Effluent
time Temperature Volume Volume Density Solute
time Solute Volume
(min) (oC) (mL) (mL) (g/mL) Composition
(min) (g) (mL)
10 30
30 30
10 50
30 50

35
Appendix 3
Type of solute =
Type of solvent =
Heating temperature = __________oC
Vacuum pressure = ____________ mbar
Circulation flow rate = ____________ L/hr
Initial volume of feed solution = ____________ L
Initial solute concentration = ____________ g/L
Time for crystal formation = ____________ min
Initial condensate volume = ____________ L

Heat Transfer
Amount Crystal
Condensate Fluid Slurry Solution Sample
Time of Concent Yield
Volume Temperature Temperature (oC) volume
(min) Crystals ration (%)
(mL) (oC) (mL)
(g) (g/L)
Inlet Outlet Inlet Outlet

Volume of slurry collected = __________ L

Appendix 4

Low Fat High

Type of milk Full Cream Milk Fresh Milk
Calcium Milk
Initial volume (mL)
Cream volume (mL)
Cream mass (g)
Skimmed milk volume (mL)
Skimmed milk mass (g)
Percentage of cream in milk
(%)

Appendix 5
Process: ________________
Membrane Used: ___________
Test Solution: __________________

DP = 10 DP = 15 DP = 20 DP = 25
Time V C C C C
V (mL) V (mL) V (mL)
(min) (mL) (mS/cm) (mS/cm) (mS/cm) (mS/cm)
1
2
3
4
5

36
 6
7
8
9
10
11
12
13
14
15

V: Volume of collected permeates

C: Conductivity

Appendix 6.1: Table of Refractive Index

Volume (mL) Mass Fraction Refractive
Ethanol Water Ethanol, XEt Water, Xw Index

Appendix 6.2: Temperature data

Reflux (%) 100% 90% 80% 70% 60% 50%
T1 (oC)
T2 (oC)
T3 (oC)
T4 (oC)
T5 (oC)
T6 (oC)
T7 (oC)
T8 (oC)
T9 (oC)
T10 (oC)
T11 (oC)
T12 (oC)
T13 (oC)

Appendix 6.3: Product composition

Initial refractive index =
Initial Temperature =
Top Product
Refractive index
Composition
(%wt)
Bottom Product
Refractive index
Composition
(%wt)

37
Appendix A1
Binodal composition for acetone-toluene-water system

38
Appendix A2
Tie line composition for acetone-toluene-water system

39
Appendix A3
Typical calibration data for acetone-toluene-water system

40
Appendix A4
Triangular plot for acetone-toluene-water system

41
Appendix A5
Physical properties of several components

Property KCl NaCl KNO3

Name of salt Potassium Sodium Potassium
chloride chloride nitrate
Molecular weight
74.55 58.45 101.1
(g/mol)
Density (g/mL) 1.984 2.163 2.11
Normal melting point
790 800.4 333
(oC)
Normal boiling point
1420 1413 400
(oC)

42
Appendix A6
Solubility curve of various salts in water

43
Appendix A7
Specific heat capacity of water-antifreeze solutions

Specific Heat
Capacity ANTI-FREEZE = Ethylene Glycol Solution (% by volume)
(J / g / ° C)
Temperature (° C) 25 30 40 50 60 65 100
-40 4.19 4.19 4.19 4.19 2.85 2.94 4.19
-18 4.19 4.19 3.47 3.27 3.03 2.93 2.26
4 3.82 3.73 3.54 3.33 3.13 3.02 2.35
27 3.86 3.78 3.60 3.41 3.21 3.11 2.47
49 3.91 3.83 3.66 3.48 3.30 3.20 2.56
71 3.93 3.87 3.73 3.56 3.39 3.29 2.68
93 3.99 3.92 3.79 3.62 3.47 3.38 2.76
116 8.37 8.37 8.37 8.37 8.37 3.47 2.88
138 8.37 8.37 8.37 8.37 8.37 8.37 2.97

Appendix A8
Ethanol-water vapor liquid equilibrium data at 1 atm

Liquid Vapour
Composition Composition Temperature, °C
Ethanol Water Ethanol Water
0.0000 1.0000 0.0000 1.0000 100.0
0.0190 0.9810 0.1700 0.8300 95.5
0.0721 0.9279 0.3891 0.6109 89.0
0.0990 0.9034 0.4375 0.5625 86.7
0.1238 0.8762 0.4704 0.5296 85.3
0.1661 0.8339 0.5089 0.4911 84.1
0.2337 0.7663 0.5445 0.4555 82.7
0.2608 0.7392 0.5580 0.4420 82.3
0.3273 0.6727 0.5826 0.4174 81.5
0.3965 0.6035 0.6122 0.3878 80.7
0.5198 0.4802 0.6599 0.3401 79.7
0.5732 0.4268 0.6841 0.3159 79.3
0.6763 0.3237 0.7385 0.2615 78.7
0.7472 0.2528 0.7815 0.2185 78.4
0.8943 0.1057 0.8943 0.1057 78.2
1.0000 0.0000 1.0000 0.0000 78.3

44