1.

0 Introduction

Separations by the use of membranes are becoming increasingly important in the process
industries. Separation is achieved by selectively passing (permeating) one or more
components of a stream through the membrane while retarding the passage of one or more
other components. Membranes can selectively separate components over a wide range of
particle sizes and molecular weights, from macromolecular materials such as starch and
protein to monovalent ions. Membranes have gained an important place in chemical
technology and are used in a broad range of applications.

Membrane separations represent a new type of unit operation. 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, two gas phases, or a liquid and a
gas phase. The two fluid phases are usually miscible and the membrane barrier prevents
actual, ordinary hydrodynamic flow.

In membrane separation, spent metal removal fluids are pumped from a process tank
at a moderate pressure (typically 30 to 50 PSIG) and rapid flow to a series of membranes.
This flow is typically between 750 to 1,100 gallons per square foot of membrane per day and
is referred to as the feed rate. Large molecules and virtually all petroleum products are
blocked at the membrane surface. The compounds that do not pass through the membrane are
referred to as the reject. The water-like solutions that pass through the membrane are referred
to as the "permeate".

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 membrane and removed in the retentate or passed through the
membrane in the permeate.

There are 3 different mechanisms by which membrane can perform separations:

By having holes or pores which are of such a size that certain species can pass
through and others cannot. This mechanism is called size exclusion.
By selective retardation by the pores when the pore diameters are close to
molecular sizes. This mechanism is called pore flow.
By dissolution into the membrane, migration by molecular diffusion across the
membrane, and re-emergence from the other side called solution diffusion.

Although the major uses of membranes are in the production of potable water and
separation of industrial gases, they can be used for many other important applications such as
filtration of particulate matter from liquid suspensions, air or industrial flue gas and the
dehydration of ethanol azeotropes. More specialised applications include ion separation in
electrochemical processes, dialysis of blood and urine, artificial lungs, controlled release of
therapeutic drugs and membrane-based sensors.

2.0 Objectives

The aim of this experiment is to study the characteristics of membrane by performing a

characteristics study on 4 different types of membrane.

3.0 Theory

Membrane separation is a technology which selectively separates (fractionates) materials via

pores and/or minute gaps in the molecular arrangement of a continuous structure. Membrane
separations are classified by pore size and by the separation driving force. These
classifications are
 Microfiltration (MF)
Ultrafiltration (UF)
Nanofiltration (NF)
Reverse Osmosis (RO).

Figure 3.1: Examples of variant substances shown in approximate

correspondence to the pore size of the membrane separation method that may
be employed.

Microfiltration (MF) refers to membranes system which operates at between 0.1 to 0.5
bars. Microfiltration process is a physical sieving separation technique that can be used to
remove particles and suspended solids from for colloidal and suspended solutions. Two
distinct flow configurations are commonly employed for microfiltration systems are cross
flow microfiltration and dead end microfiltration. Secondary treated effluents are passed
through semi-permeable membrane separating the suspended particles, bacteria and
microorganisms among others. Cross flow membranes are used and the suspended particles
in the range of 0.05 to 10 microns can be removed. These membranes are used as a pre-
treatment to desalination technologies such as reverse osmosis and nanofiltration and also to
remove turbidity from the fluid. Microfiltration has too many small applications; essentially it
is a sterile filtration with pore size 0.1 to 10.0 microns, this range of pore size cannot let
microorganisms to pass through. Membrane microfiltration is used in various sectors such as
Pharmaceutical, Food and Beverage, Semiconductor, Laboratory and others.

Figure 3.2: The process of microfiltration

Ultrafiltration (UF) refers to membranes having pore diameters in the range 20-1000
which is a pressure-driven purification process. Ultrafiltration is mainly used to separate a
mixture which consists of desirable and undesirable components. This process operates
between 2-10 bars but in some cases it goes up to 25-30 bar. Ultrafiltration system can be
based on hollow fibre, spiral wound or plate and frame membranes. It can be used to filter
dissolved macromolecules, such as proteins and polymers, from solution. Ultrafiltration
involves the use of a sieving mechanism to separate components. The difference between
ultrafiltration and microfiltration is in the particle size of the components that can be filtered:
ultrafiltration retains particles smaller than 0.1 micrometres in diameter. Industries such
as chemical and pharmaceutical manufacturing, food and beverage processing, and waste
water treatment, employ ultrafiltration in order to recycle flow or add value to later products.
Blood dialysis also utilizes ultrafiltration.
 Figure 3.3: The process of microfiltration

Nanofiltration is a membrane filtration-based method that uses nanometer sized

cylindrical through-pores that pass through the membrane at 90. Nanofiltration membranes
have pore sizes from 1-10 nanometers, smaller than that used
in microfiltration and ultrafiltration, but just larger than that in reverse osmosis. Membranes
used are predominantly created from polymer thin films. Materials that are commonly used
include polyethylene terephthalate or metals such as aluminum. Pore dimensions are
controlled by pH, temperature and time during development with pore densities ranging from
1 to 106 pores per cm2. Membranes made from polyethylene terephthalate and other similar
materials, are referred to as track-etch membranes, named after the way the pores on the
membranes are made. Tracking involves bombarding the polymer thin film with high
energy particles. This results in making tracks that are chemically developed into the
membrane, or etched into the membrane, which are the pores. Membranes created from
metal such as alumina membranes, are made by electrochemically growing a thin layer of
aluminum oxide from aluminum metal in an acidic medium.
 Figure 3.4: The process of microfiltration

Reverse osmosis (RO) is a water purification technology that uses a semipermeable

membrane to remove ions, molecules, and larger particles from drinking water. In reverse
osmosis, an applied pressure is used to overcome osmotic pressure, a colligative property,
that is driven by chemical potential differences of the solvent, a thermodynamic parameter.
Reverse osmosis can remove many types of dissolved and suspended species from water,
including bacteria, and is used in both industrial processes and the production of potable
water. 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. 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 solvent molecules) to pass freely. One of the most known applications
using reverse osmosis process is drinking water purification.

Figure 3.5: The process for reverse osmosis

4.0 Material and Apparatus

i. Material
Water
100 g of sodium chloride
ii. Apparatus
SOLTEQ Membrane Test Unit Model TR-14
Digital weighing balance
Stopwatch
Product tank

5.0 Procedures

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

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 control 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 maximum
(step 2) Valves Control Valve inlet pressure (bar)
1 V2,V5,V7,V11 Open V19 and V15 18
and V15 close V11
2 V2,V5,V8,V12 Open V20 and V16 12
and V16 close V12
3 V2,V5,V9,V13 Open V21 and V17 10
and 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

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).
6.0 Results

Time Weight of Permeates (g)

(min) Membrane 1 Membrane 2 Membrane 3 Membrane 4
1 59.32 71.87 40.32 418.38
2 101.60 139.64 75.82 822.66
3 143.96 200.81 112.00 1240.20
4 187.07 270.49 147.08 1666.09
5 230.41 303.40 183.22 2031.17
6 281.81 399.38 217.69 2509.58
7 334.98 461.74 257.40 2598.88
8 387.00 529.95 287.55 3018.62
9 440.02 594.80 332.69 3422.45
10 497.81 659.12 358.51 3841.96

Weight of membrane permeates (g) vs Times (min)

6000

5000
Weight of Permeates (g)

4000 Membrane 4
Membrane 3
3000
Membrane 2

2000 Membrane 1

1000

0
1 2 3 4 5 6 7 8 9 10
Times (min)

Figure 6.1: The graph weight of permeates (g) vs time (min)

7.0 Discussion

In this experiment, the main objective is to characterize the differences between 4 types of
membranes which are the (1) Microfiltration, (2) Ultrafiltration, (3) Nanofiltration and (4)
Reverse osmosis. The apparatus used to achieve the objective of this experiment 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.

Sodium chloride is used to pump from feed tank and pass through each membrane.
The weight of permeate collected was recorded in order to determine its type of membrane
and shows its efficiency for each of the membrane. The experiment started with sodium
chloride passes through membrane 1 with pressure inlet of 18 bar. The weight of permeates
were recorded each minutes until 10 minutes. For membrane 1, the weight of permeates
collected was 497.81g. Then, the experiment is continued for membrane 2 with pressure inlet
of 12 bar. For membrane 2, the weight of permeates collected after 10 minutes was 659.12g.
The experiment is continued by decreasing the pressure inlet to 10 bar for membrane 3. The
weight of permeates collected after 10 minutes using membrane 3 was 358.51g. Lastly,
sodium chloride passes through membrane 4 with pressure inlet of 8.5 bar and the weight of
permeates collected after 10 minutes was 3841.96g.

It can be concluded that for membrane 3 has the lowest weight of permeates. Thus, it
is nanofiltration process. The size of pores open for the permeates to flow is limited to 0.01-
0.001m. For membrane 4, it collected the most permeates thus it is microfiltration with sizes
of pores open is in the range of more than 0.02mm. For membrane 2, the membrane used is
ultrafiltration with 0.1-0.01mm for the range of sizes pores open. For membrane 1, it used
reverse osmosis membrane. The size of pores open is in the range of less than 0.001mm.
 From the graph plotted, it can be seen that the weight of permeates is proportionate
with time. The relationship that can be concluded is the higher the time, the higher the weight
of permeates. From the graph, the line for membrane 4 is the highest while the line for
membrane 3 is the lowest.

8.0 Conclusion

From this experiment, it can be shown that the weight of permeates differ from membrane to
membrane 4 due to different maximum inlet pressure of each membrane. The highest amount
of permeate at product is 3841.96 g and the lowest is about 358.51 g. Membrane 4 has
collected the highest weight of permeates while membrane 4 is the lowest. This shows that
separation happens rapidly at membrane 4 and slowly at membrane 3. The graph plotted
shows that weight of permeates increase with times. Throughout this experiment, it can be
concluded that every membrane will give out the same pattern at the outlet however, only the
values of the weight were different from each other. Thus, the objective of this experiment is
achieved.

9.0 Recommendation

In carried out the experiment, there are a few steps of recommendation that can be considered
in order to get accurate data and progression of the experiment runs smoothly. Firstly, during
taking the reading of weight permeates by using digital weighing balance, the reading of
weight should be taking in more significant figures to avoid any error and to get more
accurate result in order word the true values could be minimized. Plus, when taking the
weight of permeates every minutes, it is better to takes photos of the weight instead of
reading it since the weight differ every seconds due to the amount of permeates should be
recorded at the approximate moment to avoid inaccuracy.

Furthermore, the hose of collected permeates should not touch the product tank since
it will interrupt the digital weighing balance because it is very sensitive. 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.

10.0 Reference

Cengel, Y.A., Ghajar, A.J., (2011). Heat and Mass Transfer Fundamentals

And Application. 629-661. New York : The McGraw-Hill Companies,Inc.

Xiujin H., (n.d.). Advanced Physico-Chemical Treatment Process. 125-129.

Mcllvaine, Robert. "Reverse Osmosis" Chemical Engineering. August 2008: page 20

24.

Membrane Separation Technology Primer: Principle of Membrane Separation by

Pressure. Retrieved 2 May 2016 https://www.asahi
kasei.co.jp/membrane/microza/en/kiso/kiso_2.html

R.D.Noble, S.A.Stern, (2003). Membrane Separation Technology: Principles

and Applications. Page 1-74. Elsevier Amsterdam, The Netherlands.

11.0 Appendix