UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

CHEMICAL ENGINEERING LABORATORY 2 (CHE 523)
NAME
GROUP
EXPERIMENT
SEMESTER
PROGRAMME / CODE
LECTURER
No.

Title

: MUHAMMAD SOLAHUDIN BIN MUSA

: EH 220 3
: LAB 6: MEMBRANE SEPARATION
:3
: EH220
: MADAM NURHASLINA CHE RADZI
Allocated Marks (%)

Abstract/Summary

Introduction

Aims

Theory

10

Apparatus

Methodology/Procedure

10

Results

10

Calculations

10

Discussion

20

10

Conclusion

11

Recommendations

12

Reference / Appendix

10

TOTAL MARKS

100

Remarks:

Checked by :

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

Marks

Date : 1.0 ABSTRACT

The experiment is carried out 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) 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 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

Figure 2.2: Comparison for 4 types of membranes

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

Membrane
Membrane
Membrane
Membrane

1:
2:
3:
4:

AFC 99 (polyamide film)

AFC 40 (polyamide film)
CA 202 (cellulose acetate)
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% CaCl 2 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 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

In
permeate

of membrane
reverse

is

about 1 atm, and very high

nearly

pure

osmosis,
water

at

pressure is applied to the feed

solution to make 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 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.

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.

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 increase. This is due to the fouling effect that occurs inside
the

membrane

and

will

cause

increases

expenditure, reduce flux, membrane failure.

pressure

drop,

increases

energy

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

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), IonExchange (IE) and Reverse Osmosis (RO).

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.

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)

TR 14 model (membrane test unit)

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

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

6.0 PROCEDURES
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.
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

Retentate

Membrane

(step 2)

Valves

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

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)
Membrane 1
1
2
3
4
5
6
7
8
9
10

Max P=18
49.07
95.57
138.60
182.57
225.00
267.79
312.23
356.68
401.99
446.00

Weight of Permeates (g)

Membrane 2 Membrane 3
Max P=12
70.95
134.80
198.53
261.90
325.20
389.30
459.63
519.49
582.07
647.58

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

Membrane 4
Max P=8.5
559.16
1168.04
1779.58
2386.42
2974.54
3587.32
4194.05
4802.24
5622.92
6221.85

8.0 CALCULATION

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.
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 m 3, 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.

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.

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 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

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

Figure 13.2 :The figure shown that jars and Digital weighing balance