UNIVERSITI TEKNOLOGI MARA

HEAT AND MASS TRANSFER LABORATORY / CHE504

NAME : MOHD YASHFI BIN MOHD YUNUS / 2016238952

EXPERIMENT : MEMBRANE SEPARATION
DATE PERFORMED : 4 APRIL 2018
SEMESTER :4
PROGRAMME : BACHELOR (HONS) CHEMICAL ENGINEERING / EH 220
GROUP : EH2204D / GROUP 2
LECTURER : MADAM ROHANI

NO TITLE ALLOCATED MARKS

MARKS (%)

1. ABSTRACT / SUMMARY 5

2. INTRODUCTION 5

3. AIMS / OBJECTIVES 5

4. THEORY 5

5. APPARATUS 5

6. PROCEDURES 10

7. RESULT 10

8. CALCULATIONS 10

9. DISCUSSION 20

10. CONCLUSIONS 10

11. RECOMMENDATIONS 5

12. REFERENCES 5

13. APPENDICES 5

TOTAL 100

REMARKS :
CHECKED BY :

1|Page
 TABLE OF CONTENTS

TITLE PAGE

1 ABSTRACT 3

2 INTRODUCTION 3-7

3 AIMS / OBJECTIVES 7

4 THEORY 7-9

5 APPARATUS 9-11

6 METHODOLOGY / PROCEDURES 8-9

7 RESULTS 11-13

8 DISCUSSION 14-15

9 CONCLUSION 15

10 RECOMMENDATIONS 16

11 REFERENCE / APPENDICES 16-17

2|Page
1.0 ABSTRACT

The experiment is carried out to study on four different types of membrane by using
Membrane Unit Test Model TR14. The experiment is conducted to study characteristic
based on 4 types of membrane which are AFC99 (polymide film), AFC40 (polymide
film), CA 202 (cellulose acetate) and FP 100 (PVDF), by using Membrane Unit.
Moreover, this experiment was run to determine the characteristic of 4 type of
membrane in term of different pore size by separation driving forces which are reverse
osmosis (RO), nanofiltration (NF), ultrafiltration (UF) and microfiltration (MF)
membranes. For every 2 minutes until 10 minutes, the sample permeate is collected and
its weight was recorded for each type of membrane used. As the experiment running,
the solution will permeate through the membrane leaving only macromolecules behind.
The highest amount of permeates during 10 minutes intervals is 790.71g which
collected form membrane 4 and the lowest is about 143.58g collected from membrane
1. The trend of the graph of weight of permeates against time shows that for membrane
4, the line increase gradually and rapidly with increasing of time. Meanwhile, for
membrane 1, 2 and 3 the line shows sloppier with increase of the time. The experiment
is successfully conducted.

2.0 INTRODUCTION

Membrane separation is a technology which selectively separates (fractionates)

materials via pores and or minute gaps in the molecular arrangement of a continuous
structure. This technology used to enhance or replace traditional method of gas
purification. David and Sandall stated that the student should know the important of
this separation include understand the objective which is include an inverse mass
transfer analysis of experimental data for key membrane transport parameter.

In this experiment, Membrane Test Unit Model TR 14 has been designed to

demonstrate the technique of membrane separations which has become highly popular
as they provide effective separation without the use of heating energy as in distillation
processes. Heat sensitive materials, such as fruit juices, can be separated or
concentrated by virtue of their molecular weights. The unit consists of a test module
supplied with four different pressure membranes, and also consists of four different
membranes, namely the reverse osmosis (RO), nanofiltration (NF), ultrafiltration (UF)
and microfiltration (MF) membranes. The unit is suitable for carrying out a wide range
of experiments such as:

3|Page
  Dewatering
 Concentration
 Demineralisation
 Sugar removal
 Clarification
Reverse osmosis is one of the types of membrane separation process. This
membrane separation process impedes the passage of low molecular weight solute
which is placed between a solute-solvent solution and a pure solvent. The solvent
diffuses into the solution by osmosis. In reverse osmosis, a reverse pressure difference
is imposed which causes the flow of solvent to reverse, as in the desalination of
seawater. This process is also used to separate other low molecular weight solutes, such
as salts and sugars.

Other type of membrane separation process is ultrafiltration. This process use

pressure to obtain a separation of molecules by means of semipermeable polymeric
membrane. The membrane discriminates on the basis of molecular size, shape or
chemical structures and separates relatively high molecular weight solutes such as
proteins, polymers and colloidal materials. The osmotic pressure is usually negligible
because of high molecular weights.

Microfiltration is also one of the membrane separation processes. In

microfiltration, pressure-driven flow through the membrane is used to separate micron-
size particles from fluid. The particles are usually larger than those in ultrafiltration.
Examples are separation of bacteria, paint pigment, yeast cells, and so on from
solutions.
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

4|Page
energy as in distillation process, sublimation or crystallization . This type of membrane
is mostly used among industry in biotechnology and process industry.

Figure Above:- 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

5|Page
 Figure Above: 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 800C whereas the AFC 40 has 60% CaCl2 rejection at 60 bar
and 600C 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 300C 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

6|Page
 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.

3.0 OBJECTIVE

The experiment is conducted in order:

 To study the characteristics of membrane by performing a characteristic study

on 4 different types of membranes.

4.0 THEORY

Membrane separation processes have very important role in separation industry.

Nevertheless, they were not considered technically important until mid-1970.
Membrane separation processes differ based on separation mechanisms and size of the
separated particles. The widely used membrane processes include microfiltration,
ultrafiltration, nanofiltration, reverse osmosis, electrolysis, electro dialysis, gas
separation, vapor permeation, pervaporation, membrane distillation, and membrane
contactors. All processes except for pervaporation involve no phase change. All
processes except (electro) dialysis are pressure driven. Microfltration and ultrafiltration
is widely used in food and beverage processing (beer microfiltration, apple juice
ultrafiltration), biotechnological applications and pharmaceutical industry (antibiotic
production, protein purification), water purification and wastewater treatment,
microelectronics industry, and others. Nanofiltration and reverse osmosis membranes
are mainly used for water purification purposes. Dense membranes are utilized for gas
separations (removal of CO2 from natural gas, separating N2 from air, organic vapor
removal from air or nitrogen stream) and sometimes in membrane distillation. The later
process helps in separating of azeotropic compositions reducing the costs of distillation
processes.

7|Page
 Membrane separation is a technology which fractionates materials through
pores and minutes of gaps in the molecular arrangements of a continuous structure.
Membrane separation can be classified by pore size and by the separation driving force
likes below.

Figure Above : This figure is examples of different substance that

correspondence to the pore size of the membrane separation method.

This figure is examples of different substances that correspondence to the pore

size of the membrane separation method. Ultrafiltration enables precise separation,
concentration and purification of dissolved and suspended constituents based on the
relative molecular size of substances. Microfiltration membranes enable efficient and
precise separation as well as concentration of suspended and colloidal particles.
Reverse osmosis separates aqueous ionic solutions of different concentration. There is
an osmotic pressure when the solvent moves from an area of high water potential to
low water potential so that equal ionic concentrations on each side of membranes.

8|Page
5.0 APPARATUS AND MATERIALS

1) TR 14 model (membrane test unit)

2) Digital weighing balance
3) Jars
4) Stopwatch
5) 20 L of tap water
6) Sodium chloride solution
water

Figure Above:The figure shown that Membrane Test Unit model TR14

9|Page
 Figure Above: Pressure gauge of the unit membrane.

Figure Above: Equipment control panel and Valve

10 | P a g e
 Figure Above: Location of 4 type of membrane

6.0 PROCEDURES

6.1 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

6.2 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.

11 | P a g e
 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 Retentate Membrane
(step 2) Control Valve maximum inlet
pressure (bar)
1 V2,V5,V7,V11 and Open V19 and V15 18
V15 close V11
2 V2,V5,V8,V12 and Open V20 and V16 12
V16 close V12
3 V2,V5,V9,V13 and Open V21 and V17 10
V17 close V13
4 V2,V5,V10,V14 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.

12 | P a g e
 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 Membrane 3 Membrane 4
Max P=18 Max P=12 Max P=10 Max P=8.5
1 60.01 126.50 73.97 742.21
2 116.86 243.73 142.76 1078.23
3 182.31 360.25 209.30 1404.69
4 245.27 467.75 275.30 1721.70
5 305.31 595.52 338.51 2041.02
6 370.21 713.91 400.31 2406.76
7 430.14 841.49 460.12 2726.84
8 491.27 969.54 520.05 3479.38
9 549.26 1097.11 579.28 3862.25
10 614.63 1227.01 636.87 4154.58
TOTAL 3365.27 6642.81 3636.47 23617.66

13 | P a g e
 Membrane of permeatage(g) versus time(min)
4500
4000
Membrane permatage(g)

3500
3000
2500
2000
1500
1000
500
0
1 2 3 4 5 6 7 8 9 10
Time(min)

Membrane 1(P=18) Membrane 2(P=12) Membrane 3(P=10) Membrane 4(P=8.5)

8.0 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.

14 | P a g e
 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 614.63g. The pressure is
decrease to 12 bar for the membrane 2 and permeate collected is 1227.01 g after 10
minutes. Lowest pressure was set for membrane 4 which is only 8.5 bar and
highest permeate is recorded for about 4154.58 g. However, when the pressure is
10 bar for the membrane 3, permeate collected is 636.87 g after 10 minutes.

9.0 CONCLUSIONS

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 4154.58 g and the lowest is about 614.63 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 third 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. Thus, it shows that membrane 1 shows reverse osmosis filtration,
membrane 2 which is second highest is nanofiltration, membrane 3 which is the
lowest is ultrafiltration and membrane 4 which is the highest is microfiltration.
Therefore, the objectives of this experiment are successfully achieved.

15 | P a g e
10.0 RECOMMENDATIONS

 General step-up must be conducted as given then followed by the experiment

procedures and end with the general shut-down procedures.

 During taking the weight of permeates by using digital weighing balance, the reading
should be taking in more significant figures so that the reading of the actual weight of
permeates are more accurate and the value of true error could be minimized.

 To collect sample, the sampling valves should be open and close simultaneously so
that there is no interruption during collecting the sample.

 The system should be run in more than 5 minutes so that the system and membrane
maximum inlet pressure is more stabilized in order to get the accurate value of
weight.

 The average weight of permeates should be calculated by taking the weight of

permeates in 3 times in order to get more accurate value of weight.

11.0 REFERENCES
 Equipment for Engineering Education & Research MEMBRANE ... (n.d.). Retrieved
April 13, 2016, from http://www.solution.com.my/pdf/TR14(A4).pdf

 What is membrane separation ? (n.d.). Retrieved March 29, 2016, from

https://www.asahi-kasei.co.jp/membrane/microza/en/kiso/kiso_1.html

 Membrane Technology. (n.d.). Retrieved March 29, 2016, from

https://en.wikipedia.org/wiki/Membrane_technology

 http://www.lenntech.com/membrane-technology.htm ,Retrieved at 24/5/2014

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

Engineering, McGraw-Hill,7th Edition

 https://www.coursehero.com/file/9382641/membrane-seperation-unit-lab/

 https://www.scribd.com/document/248186195/Full-Membrane-Separation

16 | P a g e
12.0 APPENDICES

17 | P a g e