UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

PROCESS ENGINEERING LABORATORY II
(CPE 554)
NAME

GROUP

: EH 221 (4B) GROUP 4

EXPERIMENT

: MEMBRANE SEPARATION

DATE PERFORMED

: 16/5/2014

SEMESTER

:4

PROGRAMME CODE

: EH221 BACHELOR (HONS) OF CHEMICAL AND

PROCESS AND ENGINEERING

SUBMIT TO

: MADAM SITI SHAWALIAH IDRIS

DATE SUBMITED

: 2 /5/2014

No
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Title
Abstract/Summary
Introduction
Aims
Theory
Apparatus
Methodology/Procedure
Results
Calculations
Discussion
Conclusion
Recommendations
Reference
Appendix

Allocated marks (%)

5
5
5
10
5
10
10
10
20
5
5
5
5
100

TOTAL MARKS
Remarks:
Checked by:
________________
Date:

TABLE CONTENT
Number

Title

Pages

Marks

MEMBRANE SEPARATION UNIT

1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.

Abstract/Summary
Introduction
Aims
Theory
Apparatus
Methodology/Procedure
Results
Calculations
Discussion
Conclusion
Recommendations
Reference
Appendix

3
4-8
9
10-13
14
15-16
17
17
18-19
20
21
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22-24

1.0 ABSTRACT
The experiment is carried our to study on four different types of membranes by using
Membrane Test Unit model TR14.The experiment is conducted to study characteristics based
on 4 different types of membrane which are AFC99(polyamide film),AFC 40 (polyamide
film),CA 202 (cellulose acetate) and FP 100 (PVDF),by using Membrane Test Unit model
TR14. In plus, this experiment was made to determine the characteristics of 4 types of
membranes which different in term of pore size by separation driving force is namely as
reverse osmosis (RO), nanofiltration (NF), ultrafiltration (UF) and microfiltration (MF)
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MEMBRANE SEPARATION UNIT

membranes. Besides that, another aim in this experiment is to calculate the composition of
solid salt at product. The experiment was run using approximately sodium chloride solution.
The pressure supply for each membrane is different at maximum pressure for at which is 18
bar, 12 bar, 10 bar and 8.5 bar for membrane 1, 2, 3, and 4 respectively. For every 1 minute to
10 minutes, the permeate sample is collected and its weight was recorded for each type of
membrane use. As the experiment goes, the solution will permeate through the membrane
leaving only macromolecules behind. The sample of permeates were taken too made up the
weight of permeates per time. The highest amount of permeate during 10 minutes is 6221.85
g that is for membrane 4 and the lowest is about 325.53 g that is membrane 1. The graph of
permeate weight versus time then is plotted. From the graph, when the time increase, the
permeate weight also increases. For the membrane 4, the line increases gradually. For the
membrane 1, 2 and 3 the lines show sloppier with increase in the percentage of composition
of salt at product. The experiment was completely and successfully conducted.

2.0 INTRODUCTION
In our real life, the membrane technology is mostly used in transport of substances
between two fractions with the help of permeable membranes for separation of gaseous or
liquid streams .Membrane technology are available in variety of separation capabilities have
become the technology .It used not only removal of turbidity, precursors, microorganism
relating to underground , surface water supplies and other. But for our experiment, the
Membrane Test unit Model TR 14 shown in Figure 2.1 has been designed to demonstrate the
technique of membrane separations which highly popular as they provided effective
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MEMBRANE SEPARATION UNIT

separation without the use of heating energy as in distillation process, sublimation or
crystallization . This type of membrane is mostly used among industry in biotechnology and
process industry.

Figure 2.1:- Membrane Test unit Model TR 14

This self- contained unit on a mobile epoxy coated steel framework, it requires only
connection to a suitable electricity supply and a normal cold water supply to be fully
operational. It consists of a feed tank, a product tank, a feed pump, a pressure regulator, a
water bath, and a membrane test module. All parts in contact with the process fluid ate
stainless steel, PTFE, silicone rubber or nitrile rubber. The unit comes with a high pressure
feed pump for delivering the feed to the membrane unit at the desired flow rate and pressure.
The retentate line can be either returned to the feed tank or straight to the drain. Appropriate
sensors for flow, pressure and temperature are installed at strategic locations for process
monitoring and data acquisitions.
This TR 14 consists of a test module supplied with four different membranes, namely the
reverse osmosis (RO), nanofiltration (NF), ultrafiltration (UF) and microfiltration (MF)
membranes as shown in Figure 2.2

MEMBRANE SEPARATION UNIT

Figure 2.1: Comparison for 4 types of membranes

. The TR 14 unit is supplied with 4 membranes which are:

Membrane 1: AFC 99 (polyamide film)

Membrane 2: AFC 40 (polyamide film)
Membrane 3: CA 202 (cellulose acetate)
Membrane 4: FP 100 (PVDF)

The AFC 99 is rated with 99% NaCl rejection at maximum pressure and temperature which is
64 bar and 80 whereas the AFC 40 has 60% CaCl2 rejection at 60 bar and 60 .
Both of these membranes use in operation of reverse osmosis. Meanwhile, the CA 202 is
rated with apparent retentation of 2000 MWCO and the FP 100 is 100000 MWCO. Both of
these two membranes use in ultrafiltration process which CA 202 operates at 25 bars and 30
while the FP 100 is at 10 bar and 80 .

Many processes for separation of gaseous or liquid mixtures use semi permeable membranes
that allow one or more constituents of the mixture to pass through more readily than the
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MEMBRANE SEPARATION UNIT

others. The membrane may be thin layers of a rigid material such as porous glass or sintered
metal, but more often they are flexible films or synthetic polymers prepared to have a high
permeability for certain types of molecules.

Figure 2.3: Closed look of

membrane

In reverse

osmosis, permeate is nearly

pure water at about 1 atm,

applied to the feed solution to make

and very high pressure is

the activity of the water slightly

greater than that in permeate. This provides an activity gradient across the membrane even
through the concentration of water in the product is higher than in the feed.
There are several processes for the separation of liquid mixtures using porous membranes or
asymmetric polymer membrane. With porous membranes, separation may be depending just
on differences in diffusivity, as is the case with dialysis, where aqueous solutions at
atmospheric pressure are on both sides of the membrane. For liquid-liquid extraction using
porous membranes, the immiscible raffinate and extract phases are separated by the
membrane, and differences in the equilibrium solute distribution as well as differences in
diffusivity determine the extract composition.
Microfiltration (MF) and ultra-filtration (UF) systems used a lower pressure compare
to reverse osmosis (RO) and nanofiltartion (NF). Both the MF and UF have been shown to
exceed the removal efficiencies. MF and UF membrane system generally use hallow fibers
that can be operated in the outside in or inside out direction of flow.
In desalination, salt water on one side of a semi-permeable RO membrane is subjected
to high pressure. This cause fresh water to diffuse through the membrane and leaves behind
more concentrated solution that the source supply, containing the majority of the dissolved
minerals and other contaminants. A loose version of RO called Nanofiltration typically
operates at 85to 95% recovery, without pressures. Nanofiltration and reverse osmosis
membranes are mainly used for water purification purposes.
Reverse osmosis separates aqueous ionic solutions of different concentration. In
osmosis, solvent transports from a dilute solute or salt solution to a concentrated solute or salt
6

MEMBRANE SEPARATION UNIT

solution across a semipermeable membrane which allows passage of the solvent but impedes
passage of the salt solutes. When the solvent moves from an area of high water potential to
low water potential, there exist an osmotic pressure so that equal ionic concentrations on each
side of membranes. Water molecules will pass to dilute solution side through the membrane if
when a hydraulic pressure is applied to the concentrated solution which is greater and in
reverse to the osmotic pressure. Thus, by using this process it can be separate water from ions
and low-molecular weight organic constituents. As a result, the solute is retained on the
pressurized side of the membrane and the pure solvent is allowed to pass to the other side. To
be "selective," this membrane should not allow large molecules or ions through
the pores (holes), but should allow smaller components of the solution (such as the solvent) to
pass freely. Nanofiltration is about a process of water purification that use to remove
contaminates from the water to produce clean, clear and pure water. Nanofiltration is is a
form a reverse osmosis, that function to remove bivalent hardness, calcium, and magnesium
plus sulphate but leave in most of the single valent sodium ion.
Ultrafiltration is a type of separation process by using membranes with pore sizes in
the approximately range is 0.1 to 0.001 micron. Basically, ultrafiltration mostly use by
industry is to remove high molecular-weight substances, colloidal materials, and organic and
inorganic polymeric molecules. But, the type like low molecular-weight organics and ions
such as sodium, calcium, magnesium chloride, and sulphate are not removed. Thus, this is
because ultrafiltration will remove only high-molecular weight species .To achieve high flux
rates from an ultrafiltration membrane ,then the low applied pressures are apply. Flux of a
membrane is defined as the amount of permeate produced per unit area of membrane surface
per unit time.
Meanwhile, microfiltration is a membrane technical filtration process which removes
contaminants from a fluid (liquid and gas) by passage through a microporos membrane. This
type of membrane pore size range is 0.1 to 10 micrometers (m). Microfiltration is
fundamentally different from reverse osmosis and nanofiltration because those systems use a
pressure as a means of forcing water to go from low pressure to high pressure. Microfiltration
can use a pressurized system but it does not need to include pressure.

MEMBRANE SEPARATION UNIT

3.0 OBJECTIVES
The experiment is conducted in order:

To study the characteristics of membrane by performing a characteristic study on 4

different types of membranes.

To calculate the composition of solid salt at product.

MEMBRANE SEPARATION UNIT

4.0 THEORY
There are several types of equipment for membrane processes. The membrane acts as
a semipermeable barrier and separation occurs by the membrane controlling the rate of
movement of various molecules between two liquid phases. The two fluid phases are usually
miscible and the membrane barrier prevents actual, ordinary hydrodynamic flow. First is flat
membrane is usually to characterize the permeability of the membrane. The modules are easy
to fabricate and use and the areas of the membranes are well defined. Next, spiral wound
membranes and this configuration retains the simplicity of fabricating flat membranes while
increasing markedly the membrane area per unit separator volume. Third is hallow fibre
membranes and the membranes are in the shape at very small diameter hollow fibres.
The graph of permeate weight versus time that should we get is increase in permeate weight
as time increase. But at certain time, the curve shape will be seen as time of separation

MEMBRANE SEPARATION UNIT

increase. This is due to the fouling effect that occurs inside the membrane and will cause
increases pressure drop, increases energy expenditure, reduce flux, membrane failure.

Figure 4.1 :The figure above shown that ,the filtration range for every each type of
membrane.

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MEMBRANE SEPARATION UNIT

Figure 4.2 : The figure shown that type of membrane use to separate components.

Membrane separation can be classified by pore size and by the separation driving force for
example Microfiltration (MF), Ultrafiltration (UF), Nanofiltration (NF), Ion-Exchange (IE)
and Reverse Osmosis (RO).

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MEMBRANE SEPARATION UNIT

Figure 4.3 : This figure is examples of different substance that correspondence to the
pore size of the membrane separation method.

The membrane separation techniques utilized in the dairy industry serve different purposes:
RO mostly it used for dehydration of whey, UF permeate and condensate.
NF mostly it used when partial desalination of whey, UF permeates or retentate is
required.
UF -typically used for concentration of milk proteins in milk and whey and for
protein standardization of milk intended for cheese, yoghurt and some other products.

MF -basically used for reduction of bacteria in skim milk, whey and brine, but also
for defatting whey intended for whey protein concentrate (WPC) and for protein
fractionation.
Membrane processes are characterized by the fact that a feed stream is divided into 2
streams: retentate and permeate. The retentate is that part of the feed that does not pass
through the membrane, while the permeate is that part of the feed that does pass through the
membrane. The optional "sweep" is a gas or liquid that is used to help remove the permeate.
The component(s) of interest in membrane separation is known as the solute. The solute can
be retained on the membrane and removed in the retentate or passed through the membrane in
the permeate.

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MEMBRANE SEPARATION UNIT

Figure 4.4 : This figure is process of membrane technology
Some components are allowed passage by the membrane into a permeate stream,
whereas others are retained by it and accumulate in the retentate stream. Some advantages of
membrane separation are less energy-intensive, since they do not require major phase
changes, do not demand adsorbents or solvents, which may be expensive or difficult to
handle and the equipment simplicity and modularity, which facilitates the incorporation of
more efficient membranes. The particular advantage of membrane separation processes is that
it operate without heating and thus are energetically usually lower than conventional thermal
separation processes (distillation, Sublimation or crystallization).

5.0 APPARATUS AND MATERIALS

1)
2)
3)
4)
5)
6)
7)

13

TR 14 model (membrane test unit)

Digital weighing balance
Jars
Stopwatch
20 L of tap water
Sodium chloride solution
water

MEMBRANE SEPARATION UNIT

Figure 5.1:The figure shown that Membrane Test Unit model TR14.

6.0PROCEDURES
6.01 General Start-Up Procedures:
1. Ensure all valves are initially closed.
2. A sodium chloride solution was prepared by adding 100 gram of sodium chloride into
20L of water.
3. The feed tank was filled up with salt solution prepared in step 2. The feed shall always
be maintained at room temperature.
4. The power was turned on for the control panel. All sensors and indicators are checked
for functioning properly.

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MEMBRANE SEPARATION UNIT

5. The thermostat was switched on and make sure the thermo oil level was above the
coil inside thermostat. Thermostat connections are checked so that they are properly
fitted.
6. The unit is now ready for experiment

6.02 Experimental Procedure:

1. The general start-up procedure was performed.
2. The experiment for Membrane 1 was started. Open valves V2, V5, V7, V11 and V15.
3. The plunger pump (P1) was switched on to set the maximum working pressure at 20
bars, and slowly close valve V5. Observe pressure value at pressure gauge and the
pressure regulator was adjusted to 20 bars.
4. Valve V5 was opened. Then, membrane maximum inlet pressure was set to 18 bars
for Membrane 1 by adjusting the retentate contral valve (V15).
5. The system was allowed to run for 5 minutes. The sample was start to collect from
permeate sampling port and the sample was weight using digital weighing balance.
The weight of permeates was recorded every 1 minute for 10 minutes.
6. Step 1 to 5 was repeated for Membrane 2, 3 and 4. Open and close the respective sets
of valves and the membrane maximum inlet pressure was adjusted for every
membrane.

7.
Membrane

Open Valves

Sampling Valves

(step 2)

Retentate

Membrane

Control Valve

maximum inlet

V2,V5,V7,V11

Open V19 and

V15

pressure (bar)
18

and V15
V2,V5,V8,V12

close V11
Open V20 and

V16

12

and V16
V2,V5,V9,V13

close V12
Open V21 and

V17

10

and V17
V2,V5,V10,V14

close V13
Open V22 and

V18

8.5

and V18

close V14

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MEMBRANE SEPARATION UNIT

8. Plot the graph of permeate weight versus time
6.03 General Shut-Down Procedure:
1. The plunger pump was switched off (P2)
2. Valve V2 was closed.
3. Drain all liquid in the feed and product tank by opening valves V3 and V4.
4. Flush all the piping with clean water. Close V3 and V4, fill the clean water to feed
tank until 90% full.
5. The system was run with the clean water until the feed tank is nearly empty this is for
cleaning purpose).

7.0 RESULTS
Time (min)

Weight of Permeates (g)

Membrane 1
Membrane 2

Max P=18
1
49.07
2
95.57
3
138.60
4
182.57
5
225.00
6
267.79
7
312.23
8
356.68
9
401.99
10
446.00
8.0 CALCULATION

16

Max P=12
70.95
134.80
198.53
261.90
325.20
389.30
459.63
519.49
582.07
647.58

Membrane 3

Membrane 4

Max P=10
32.09
57.65
89.91
121.73
155.67
190.73
223.47
257.20
291.28
325.53

Max P=8.5
559.16
1168.04
1779.58
2386.42
2974.54
3587.32
4194.05
4802.24
5622.92
6221.85

MEMBRANE SEPARATION UNIT

Membranes of permeate(g) versus time(min)

7000
6000
5000
Membrane 1(P=18)

4000
Membranes of permate(g)

Membrane 2(P=12)
3000

Membrane 3(P=10)
Membrane 4(P=8.5)

2000
1000
0
0

10

12

Time(min)

9.0 DISCUSSION
In this experiment, we were to characterize the differences between four types of
membranes, which are the reverse osmosis (RO), nanofiltration (NF), ultrafiltration (UF), and
microfiltration (MF). In doing this experiment, the apparatus used to accomplish the objective
is SOLTEQ Membrane Test Unit (Model: TR14). This unit has been designed to demonstrate
the technique of membrane separations which has become highly popular as it provide
separation in effective way without using heat energy as used in distillation process. Heat
sensitive materials, such as fruit juices can be separated or concentrated by virtue of their
molecular weight.Membrane separation is a process of which a solution sample and water is
run through a semi permeable membrane that allows them to separate. The separated water
will equilibrate the system, which is commonly known as osmotic pressure. When a
mechanical force is applied to exceed the osmotic pressure, the water is forced to move from
low concentration to higher concentration. Permeates designates the liquid passing through
the membrane and retentate, or concentrate designates the fraction to not pass through the
membrane.

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Thus, sodium chloride is used to pump from feed tank and pass through each
membrane and the weight of permeate collected was recorded. The weight of permeate
collected shows the efficiency for of each the membrane. The experiment is started with
sodium chloride was passed through membrane 1 with the pressure inlet of 18 bar. After 10
minutes, permeate collected is 446.00g. The pressure is decrease to 12 bar for the membrane
2 and permeate collected is 647.58 g after 10 minutes. Lowest pressure was set for membrane
4 which is only 8.5 bar and highest permeate is recorded for about 6221.85 g. However, when
the pressure is 10 bar for the membrane 3, permeate collected is 325.53 g after 10 minutes.
Second objective of this experiment is to determine the composition of solid salt at
product. With same amount of salt at the feed which is 0.02 m3, but due to the difference in
pressure for each membrane results in difference amount of permeate flowed. The
composition of salt at product is not same for the each type of membrane. This is because of
the effectiveness of each membrane it has. For example, type of material they use, the
membrane may be thin layers of a rigid material such as porous glass or sintered metal, but
more often they are flexible films or synthetic polymers prepared to have a high permeability
for certain types of molecules
Overall, from all 4 membranes, membrane 3 has lowest amount of permeates which is
only 325.53 g. While amount of permeate of membrane 4 is the highest with 6221.85 g. This
is due to the difference in pressure supply to the system and the size of pore depends on the
type of membrane used. Pressure inlet for membrane 1 is the highest with 18 bar and
membrane 4 is lowest with 8.5 bar. Also depending to the flow rate, if the flow rate is slower,
then the solution has more time to permeate. The solution will not react thoroughly with the
pore and it also caused the solution difficult to pass through the pore, size of pore in
membrane also can effect amount of permeate collected. If the size of pore is too small, the
solution cannot pass through the pore and amount of permeates also will less.
The graph plotted shows that the permeates weight is proportional with the time.
When the time is increases, the permeates weight also increasing. Besides that, the highest
line from the graph is during the membrane 4 and the lowest line is when the membrane 3 is
using. While conducting this experiment, there must be theoretical errors. General step up
must be conducted as given to ensure that the experiment can be run smoothly and are save to
use. When taking the reading, the observer must be faster because the value changes as fast as
the flow of permeates. The jar used must be clean and dry to avoid inaccurate data.
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10.0 CONCLUSION
This experiment was a quite success and conclusions can be made. Firstly, based on
the theory, the weight of permeates collected from membrane 1 to 4 can be different due to
different maximum inlet pressure of each membrane. The highest amount of permeate at
product is 6221.85 g and the lowest is about 325.53 g. It can be seen that the forth membrane
carried the largest value of weight of the collected. This shows that every membrane will give
out the same pattern at the outlet however, only the values of the weight were different from
each other. Therefore, this shows that the separation process was the fastest in the forth
membrane and the first membrane was the slowest. From the graph, the permeate weight
increases while the time increases. For the membrane 4, the line increases steadily. For the
membrane 1, 2 and 3 the lines show sloppier with increase in the percentage of composition
of salt at product. Therefore, the objectives of this experiment are successfully achieved.

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11.0 RECOMMENDATIONS
In carried out the experiment, there are a few steps of recommendation that can be
considered in order to get accurate data and smoothly in progressing the experiment. Firstly,
general step-up must be conducted as given then followed by the experiment procedures and
end with the general shut-down procedures. This is to ensure that the experiment can be
progress successfully. During taking the reading of weight permeates by using digital
weighing balance, the reading of weight should be taking in more significant figures so that
to avoid any error and to get result more accurate in order word the true values could be
minimized. Moreover, the average weight of permeates should be calculated by taking weight
of permeates in three or two times in order to get more accurate value of result. The system
should run more than 5 minutes so that the system can work more stabilized in order to get
more accurate value of weight of permeates. During collect the samples, the sampling valves
should be open and close simultaneously and immediately so that no occur in term of
interruption during collecting samples. Besides that, leftover sodium chloride in membrane 1
should be dried first before the starting of experiment for others membrane to avoid leaking
during the experiment. Before conducting to next experiment, every each of membranes must
be cleaned before and after usage to avoid fouling which might affect the final results. The
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MEMBRANE SEPARATION UNIT

amount of permeates should be recorded at the approximate moment to avoid inaccuracy.
Furthermore, used the suitable size of jar based on the amount of permeate to avoid spillage
and affect the permeate weight of solution.

12.0 REFERENCES

CHE 554 Lab Manual

McCabe,w.L Smiths,J.C and Harriott (2001), Unit Operations Of Chemical

Engineering, McGraw-Hill,7th Edition

STI International membrane Separation Tecnologies
Ridgway, Harry F. (Ph.D) (Advanced Membrane Technologies Stanford University,
2008)
http://www.lenntech.com/membrane-technology.htm ,Retrieved at 24/5/2014
http://www.kochmembrane.com/PDFs/Membrane-Filtration-Technology---KochMembrane-Sys.aspx, Retrieved at 24/5/2014
13.0 APPENDIX

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MEMBRANE SEPARATION UNIT

Figure 13.1:The figure shown that Membrane Test Unit model TR14.

Figure 13.2:The figure shown that the location 4 type of membrane Membrane Test
Unit model TR14.

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MEMBRANE SEPARATION UNIT

Figure 13.3 :The figure shown that jars and Digital weighing balance

Figure 13.4 :The figure shown that pressure gauge of Membrane Test Unit model TR14

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MEMBRANE SEPARATION UNIT

Figure 13.5 :The figure shown that the type of valve for each type membrane 1,2,3,4 of
Membrane Test Unit model TR14

24