TABLE OF CONTENTS

No. Title Page

1 Abstract 2

2 Introduction 2

3 Aim 5

4 Theory 5

5 Apparatus 9

6 Procedures 10

7 Results 12

8 Sample of calculations 13

9 Discussions 14

10 Conclusions 15

11 Recommendation 16

12 References 16

13 Appendices 17

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1.0 ABSTRACT

Membrane separation process is the separation of molecules by the use of membranes

is relatively new separation process and becoming more crucial in our industry. The aim of
the Membrane Separation Unit experiment is to study the characteristics of membrane by
performing a characteristics study on 4 different types of membrane which are AFC 99
(Polyamide Film), AFC 40 (Polyamide Film), CA 200 (Cellulose acetate), and FP 100
(PVDF). . This experiment is conducted by using Membrane Test Unit model TR 14. This
model consists of pump, switch controller, pressure monitor, valves and discharge. Before the
experiment was started, sodium chloride solution was prepared by assistant engineer. Then,
the prepared solution was poured in the feed tank. All sensor and indicators were checked to
make sure they were function well. The maximum working pressure at 20 bars were set up
before the next procedure. The pressure supply for each membrane were set differently at
maximum pressure which are 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 weight of permeate sample were collected
and the weight were recorded for each type of membrane used. From the data obtained, the
highest amount of permeate were collected during 10 minutes is 6231.65 g for membrane 4
and the lowest is 366.68 g for membrane 1. The graph of weight of permeate against time
were plotted for every membrane. From the graph, it can be concluded that, the higher the
time, the weight of permeate also will be higher. For membrane 4, the line increase gradually
while for membrane 1, 2 and 3 the lines slow increase. The experiment was completely and
successfully conducted.

2.0 INTRODUCTION

Membrane separation process is the separation of molecules by the use of membranes

is relatively new separation process and becoming more crucial in our industry. The rate of
movement of molecules between two phases depend on the relatively thin, solid membrane. It
very useful in order to remove salt from water, to purify the gases, in food processing and so
on. The membrane acts as a semipermeable blockade and separation process take places by
the membrane controlling the rate of movement of various molecules between two liquid
phases, two gas phases, or a liquid and a gas phase. The two fluid are usually miscible and the
membrane blockade prevents actual, ordinary, hydrodynamic flow (Geankoplis, C. J. 2014).

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These are the several classification of the main type of the membrane separation:

Gas diffusion in porous solid. In this type, a gas phase is present on both sides of the
membrane, which is microporous solid.
Liquid permeation or dialysis. In this case, the small solutes in one liquid phase
diffuse readily because of the concentration differences through a porous membrane
to the second liquid or vapour phase.
Gas permeation in a membrane. The membrane in this process is mostly a polymer
such as polyamide, rubber, and it is not a porous solid.
Reverse osmosis. A membrane, which disrupt the passage of the low-molecular-
weight solute, is planted between a solute-solvent solution and a pure solvent.
Ultrafiltration membrane process. In this process, pressure is used to obtain a
separation of molecules by means of a semipermeable polymeric membrane (M2).
Microfiltration membrane process. In microfiltration, pressure-driven flow through
the membrane is used to separate micron-size particles from fluids.
Gel permeation chromatography. The porous gel retards diffusion of the high
molecular weight solutes.

In the below figure are examples of variant substances shown in approximate correspondence
to the pore size of the membrane separation method that may be employed.

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 Many industrial processes for separation of gases or liquid mixtures use
semipermeable membranes that allow one or more constituents of the mixture to pass through
more rapidly than the others. The membranes may be porous membranes- thin layers of rigid
material such as porous glass or sintered metal where the constituents diffuse from region of
high pressure through the porous of lower pressure and polymer membrane. Polymer
membrane are used widely in industrial processes.

In this experiment, the membrane separation process is using the Membrane Test Unit
(Model: TR14). This unit has been design to demonstrate the technique of membrane
separation which has become highly important in industry as it can provide efficient
separation without the use of heating energy as in distillation process. This type of membrane
extensively used in biotechnology and process industry.

The P.C.I Single-Tube Tester is designed for the economical, quick, initial evaluation
of membrane types and processes for separation and concentration at laboratory to more
detailed test work.

TR 14 unit consist of a test module supplied with four different namely, nanofiltration
(NF), ultrafiltration (UF), microfiltration (MF) and reverse osmosis (RO).

The TR 14 unit is supplied with membrane:

Membrane 1: AFC 99 (Polyamide Film)

Membrane 2: AFC 40 (Polyamide Film)
Membrane 3: CA 200 (Cellulose acetate)
Membrane 4: FP 100 (PVDF)

The AFC 99 is rated with 99% sodium chloride (NaCl) rejection and AFC 40 has 60%
calcium chloride CaCl2. The CA 200 membrane is rated with apparent retention character of
2000 MWCO while FP 100 PVDF membrane is 100000 MWCO.

3.0 AIM

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

different types of membrane.

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4.0 THEORY

Membrane separation is relatively new separation process, the membrane acts as a

semipermeable barrier and selectively separates materials by the membrane controlling the
rate of movement of various molecules via pores or minute gaps between two liquid phases,
two gas phases or a liquid and a gas phase (Geankoplis, 2014). Membrane separations take
place due to pore size and driving force transporting a compound through membrane such as
pressure and concentration differences. Liquid permeation and gel permeation
chromatography are the example of membrane separation that uses concentration differences
as driving force. Pressure driven process are including reverse osmosis, ultrafiltration and
microfiltration.

Figure 1: Membrane separation process with different driving force

There are two modes used for membrane separation which are direct flow mode and
cross flow mode. In direct flow mode, the water supply passes directly through the filter
meanwhile a cross flow mode employs high velocity of water flowing in parallel over the
membrane surface. Cross flow mode will keeps the membrane surface from forming solids or
from fouling (Asahi, 2013).

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 Figure 2: Direct flow mode

Figure 3: cross flow mode

Membrane can separate the component over a wide range of particle sizes and
molecular weight. In membrane process, the feed stream is divided into 2 streams which are
retentate and permeate. Retentate is feed that filtered from some of the pores through while
permeate is the feed that pass through the membrane (Hewitt, 2013). Permeates dissolve in
the membrane material as in a liquid and then diffuse through the membrane under any
pressure condition that can pressed permeates out of permeate porous.

Membrane separation can be divided up between microfiltration, ultrafiltration and

reverse osmosis. Microfiltration and ultrafiltration are used when the process involves
separation of larger particles. When salts need to be removed from water, reverse osmosis is
applied. Reverse osmosis required higher pressure than micro and ultra-filtration
(Geankoplis, 2014)

Reverse osmosis separates salts or small molecules from low molecular weight solute
at high pressure using membrane that is placed between a solute solvent solution and a pure

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solvent. The solvent water will flows through the semipermeable membrane to the salt
solution (Geankoplis, 2014). The solvent pressure can be reduced by applying a pressure on
the salt solution side until at certain pressure of the salt solution is reached and the amount of
solvent passing in opposite direction is equal (Geankoplis, 2014).

The most widely used reverse osmosis membrane is cellulose acetate membrane. It
have low fouling tendency, high chlorine resistance and of course a very low cost. The
asymmetric membrane is made as a composite film which is thin and dense layer that has the
ability to block passage of quite small solute molecules. Another membrane that is prevalent
with reverse osmosis is aromatic polyamides. Compared to the cellulose, aromatic
polyamides have better chemical, thermal and biological stability, however they are highly
prone to degradation in the presence of chlorine (Takeshi, 2014).

Figure 4: osmosis and reverse osmosis (a) osmosis, (b) osmotic equilibrium, (c) reverse
osmosis

Ultrafiltration is a process where solvent and small solute molecules pass through the
membrane and collected as permeate. Larger molecule do no pass through the membrane and
collected in a concentrated solution (Geankoplis, 2014). It is also used to separates mixture of
different molecular weight protein. Ultrafiltration membranes are microporous and permeable
to small solute species similar to reverse osmosis. Ultrafiltration membrane is likely to keep
large solute species in the retentate. Thus the pressure required in ultrafiltration is not as high
as the reverse osmosis. Membrane is usually made from aromatic polyamides, cellulose
nitrate or polysulfone (Geankoplis, 2014).

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 Microfiltration is used to filter micron-size of particle from fluids. The particle is
usually larger than the solutes in reverse osmosis and ultrafiltration. Thus, the osmotic
pressure can be neglect (Geankoplis,2 014). There are two types of configurations for the
microfiltration operation which are dead-end microfiltration and crossflow microfiltration.
Highly concentrated suspensions are not suitable for dead-end treatment since the separated
particle rapidly accumulate on the membrane and increase the rate of forming a clog.
Membranes that are usually used are hydrophobic and have high chemical and thermal
stability such as polytetrafluoethylene, polyvinylidene fluoride or polyethylene.

Figure 5: process flow for microfiltration; (a) dead-end flow (b) cross-flow

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5.0 MATERIAL AND APPARATUS

Apparatus:
Weighing balance

P.C.I Single-tube tester

Materials:
1. Sodium chloride solution

Membrane:
1. Membrane 1: AFC 99 (Polyamide film)
2. Membrane 2: AFC40 (polyamide film)
3. Membrane 3: CA 202 (Cellulose Acetate)
4. Membrane 4: FP 100(PVDF)

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6.0 EXPERIMENTAL PROCEDURES

6.1 General start-up Procedures

1. Ensure all valves are initially closed.

2. Sodium chloride solution was prepared by adding 100 gram of sodium chloride into
20 litre of water.
3. Sodium chloride solution prepared in step 2 was filled in the feed tank. The feed was
always maintained at room temperature.
4. All sensors and indicators were checked if they were function well after the power for
the control panel was on.
5. Thermostat was switched on to make sure the thermo oil level is above the coil inside
the thermostat.
6. The temperature at the thermostat was adjusted to maintain feed temperature.

6.2 General shut-down procedures

1. The plunger pump (P2) was switched off.

2. Valve V2 was closed.
3. All liquid in feed tank and product tank were drained by opening valves V3 and V4.
4. All the piping was flushed with clean water. Valve V3 and V4 were closed; clean
water was filled in the feed tank until 90% full.
5. For cleaning purpose, the system was operated with clean water until the feed tank is
nearly empty.

6.3 Procedure

1. General start-up procedure was performed.

2. Valves V2, V5, V7, V11 and V15 were opened to start the experiment for Membrane
1.
3. Plunger pump (P1) was switched on and valve V5 was slowly closed to set the
maximum working pressure at 20 bars. Pressure regulator was adjusted to 20 bars by
observing the pressure value at the pressure gauge.
4. The pressure regulator was adjusted by turning the adjusting screw using a proper
wrench.
5. V2 was opened to avoid operating pump in dry conditions.
6. Valve V5 was opened. Maximum Inlet pressure of the Membrane 1 was set to 18 bars
by adjusting the retentate valve (V15)
7. The system was allowed to run for 5 minutes. The sample was collected from
permeate sampling port and the sample was weighed using the digital weighing
balance. The weight of permeates was recorded every 1 minute for 10 minutes.

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 8. The sample was collected by opening Valve V19 and simultaneously closing the valve
V11.
9. Steps 1 until 5 were repeated for Membrane 2, 3 and 4. Respective sets of valves were
opened and closed. The membrane maximum inlet pressure for every membrane was
adjusted according to the table below;

Membrane Open valves Sampling Retentate Membrane

valves control valve maximum inlet
pressure (bar)
1 V2,V5,V7,V11,V15 Open V15 18
V19,close V11
2 V2,V5,V8,V12,V16 Open V16 12
V20,close V12
3 V2,V5,V9,V13,V17 Open V17 10
V21,close V13
4 V2,V5,V10,V14,V18 Open V18 8.5
V22,close V14

10. Graph of permeate weight versus time was plotted.

7.0 RESULTS

Time (min) Weight of Permeate (g)

Membrane 1 Membrane 2 Membrane 3 Membrane 4
1 39.75 64.12 64.96 478.59
2 85.88 109.90 118.91 959.10

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 3 112.32 154.47 173.48 1441.32
4 148.67 200.14 227.03 1922.41
5 184.68 245.62 281.87 2395.52
6 220.61 293.14 337.45 2618.74
7 255.36 343.97 392.67 3323.22
8 291.83 400.16 445.84 3813.04
9 326.55 457.39 500.34 4818.76
10 366.67 505.45 554.48 6231.65

MEMBRANE 1: ACF 99 (POLYAMIDE FILM)

MEMBRANE 2: ACF 40 (POLYAMIDE FILM)

MEMBRANE 3: CA202 (CELLULOSE ACETATE)

MEMBRANE 4: FP 100 (PVDF)

7000

6000

5000
membrane 1 membrane 2 membrane 3
4000

3000

2000
membrane 4
1000

0
1 2 3 4 5 6 7 8 9 10

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 Graph of weight of permeates against time

8.0 CALCULATIONS

During the experiment for membrane 4:

During the interval 6 min to 7 min, the digital weighing balance only can max up to 3100 g.
at 6 minutes the flow exceed the flow make us to plus with the previous jar.

1st jar = 3323.22g

2nd jar = 6231.65g

During the interval 2nd -1st = 6231.65 -3323.22 = 2908.43g

9.0 DISCUSSIONS

This membrane separation experiment was conducted to study the characteristics on four
different types of membranes. The membranes involved in the following experiment were
AFC 99 (Polyamide Film), AFC 40 (Polyamide Film), CA 202 (Cellulose acetate) and FP 100
(PVDF) which defined as membrane 1, 2, 3 and 4 respectively. From the obtained result, the
membranes can be classified whether as reverse osmosis (RO), nanofiltration (NF),
ultrafiltration (UF) or microfiltration (MF) membranes. Based on the graph of weight of
permeates against time that had been plotted, membrane 4 had the steepest slope followed by
membrane 3, 2 and 1.

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 From the graph, membrane 1 (AFC 99 (Polyamide Film)) can be classified as reverse
osmosis (RO) membrane. This was because it gave the lowest weight of permeates at the end
of the experiment. Impurities and particles larger than 0.001 microns would be removed by
this membrane. RO membranes are effectively non-porous therefore, only water was allowed
to pass through the dense layer, and preventing the passage of solutes (salt ions). 18 bar of
pressure was used because the process needed a high pressure, normally 2 - 17 bar for fresh
and brackish water to be exerted on the high concentration side of the membrane. This type of
membrane widely used in drinking water purification system to improve the quality of water
to be consumed.

Next, membrane 2 (AFC 40 (Polyamide Film)) showed a characteristic of

nanofiltration (NF) membrane. It operates similarly to the RO membrane however, it only
removed larger ions that made the degree of removal of monovalent ions such as chlorides
different. The membrane was porous by having pore sizes from 1-10 nanometers which was
larger than RO membrane. The membrane also applied lower maximum inlet pressure than
the RO membrane because the nanofiltration used less fine membranes. This type of
membrane usually used in water softening process, decolouring and micro pollutant removal.

Membrane 3 which is CA 202 (Cellulose acetate) had the properties of ultrafiltration

membrane. It had a pore size of around 0.1 to 0.002 micron. The particulate and microbial
contaminants would be removed, but not the ions and small molecules. Its operating pressure
usually ranging from 200 to 700 kPa. Low applied pressure was sufficient to achieve high
flux rates from the ultrafiltration membrane. Chemical and pharmaceutical manufacturing,
food and beverage production as well as water treatment were applying this ultrafiltration
membrane to add value to later products.

As for the membrane 4 (FP 100 (PVDF)), it showed the characteristic of

microfiltration membrane. It produced the highest weight of permeates from the experiment
therefore generated the steepest slope for the graph of weight of permeates against time. Its
pore size was approximately ranges from about 0.1 to 10 m. Macromolecules of molecular
weights less than 100,000 g/mol would be separated using this membrane. The membrane

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allowed more microscopic, atomic or ionic materials such as water (H2O), and monovalent
species such as Sodium (Na+) or Chloride (Cl) ions, to pass through the membrane.

10.0 CONCLUSION

After completing the experiment, the characteristics of four membranes used had been
determined. In a conclusion, membrane 1 with the lowest weight of permeates represent a
reverse osmosis membrane that operated similarly to nanofiltration membrane which was
represented by the membrane 2 with larger amount of weight of permeates. Membrane 3 with
higher amount of weight of permeates compared to membrane 1 and 2 was an ultrafiltration
membrane. Membrane 4 produced the highest weight of permeates showed that it was a
microfiltration membrane that only differed slightly in operation with the ultrafiltration
membrane.

11.0 RECOMMENDATIONS

There are many recommendations for this experiment in order to improve the result of the
experiment.

1. The weighing balance should be placed far from the pump to prevent shaking that
would affect the weight of permeates readings.
2. The readings of the weight of permeates should be taken with more significant figures
to get the more accurate values.
3. Opening and closing the valves during collecting the sample should be done
simultaneously to avoid any interruption to the collection process.
4. The pressure regulator for the previous membrane should be closed first before
opening the pressure regulator to obtain the desired maximum inlet pressure for the
next membrane.

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 5. A big container for the permeates sample should be used to avoid any spillage of the
sample.

13.0 REFERENCES

1. Hewitt, G. F. (2013). Membrane Process. Retrieved March, 23, 2016, from

http://www.thermopedia.com/editorial/
2. Baker, R. W. (2000). Membrane Technology and Research. Retrieved March 23, 2016,
from http://www.separationprocesses.com/Membrane/MT_Chp01.htm
3. Geankoplis, C.J. (2014). Transport Processes & Separation Process Principle (includes
unit operations). Pearson Education Limited.
4. Wilf M. (2008). Membrane Types and Factors Affecting Membrane Performance.
Retrieved March 21, 2016, from
http://web.stanford.edu/group/ees/rows/presentations/Wilf.pdf
5. Takeshi (2014). Membrane Separation Technologies. Retrieved March 23, 2016, from
http://www.eolss.net/eolsssamplechapters/c07/e2-14-01-02/E2-14-01-02-TXT-
02.aspx#4._Membrane_separation_processes_where_the_driving_force_is_pressure_

13.0 APPENDICES

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SOLTEQ MEMBRANE TEST UNIT (Model: TR 14)

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Description and assembly

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