INTRODUCTION

Separation by the use of membranes are becoming increasingly important in the

process industries. In this relatively new separation process, the membrane acts as a
semipermeable barrier and separation occurs by the membrane controling the rate of the
movement of various molecules between two liquid phase, 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. A classification of the main types of membrane
separation follows.

Membrane separation processes have very important role in separation industry. This
Membrane Separation Unit has been designed to demonstrate the techniques of membrane
separations which are becoming highly popular as they provide effective separation without
the use of heating energy as in distillation processes. For the mass transfer at the membrane,
two basic models can be distinguished: the solution-diffusion model and the hydrodynamic
model. In real membranes, these two transport mechanisms certainly occur side by side,
especially during the ultra-filtration. Depending on the type of membrane, the selective
separation of certain individual substances or substance mixtures is possible. Important
technical applications include drinking water by Reverse Osmosis (RO), filtrations in the food
industry, the recovery of organic vapors such as gasoline vapor recovery and the
electrolysis for chlorine production. But also in wastewater treatment, the membrane
technology is becoming increasingly important.

In this experiment, we use the SOLTEQ Membrane Test Unit (Model : TR 14) as the
device to run this experiment. This apparatus has to be desingn to demonstrate the techinuque
of membrane separations which has become hinghly popular as they provide effective
separation without the use of the heating energy in distilation process. Heat sensitive
materials, such as fruit juices can be separated or concentrated by virtue of their molecular
weights. The unit consits of a test module supplied with four different membranes, namely
Reverse Osmosis (RO), nano filtiration (NF), and microfiltration (MF) membranes

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 This self-contained unit on a mobile epoxy coated steel framework, 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 are
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.

Reverse osmosis (RO) is a membrane-technology filtration method that removes many

types of large molecules and ions from solutions by applying pressure to the solution when it
is on one side of a selective membrane. The result is that thesolute 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 describes a process of water purification that remove contaminats from

the water to produce clean, clear and pure water. Nanofiltrition is a form a reverse osmosis,
that will remove bivalent hardness, calcium, and magnesium plus sulphate but leave in most
of the single valent sodium ion.

Ultrafiltration is a separation process using membranes with pore sizes in the range of
0.1 to 0.001 micron.  Typically, ultrafiltration will remove high molecular-weight substances,
colloidal materials, and organic and inorganic polymeric molecules.  Low molecular-weight
organics and ions such as sodium, calcium, magnesium chloride, and sulfate are not removed. 
Because only high-molecular weight species are removed, the osmotic pressure differential
across the membrane surface is negligible.  Low applied pressures are therefore sufficient to
achieve high flux rates from an ultrafiltration membrane.  Flux of a membrane is defined as
the amount of permeate produced per unit area of membrane surface per unit time.  Generally
flux is expressed as gallons per square foot per day (GFD) or as cubic meters per square
meters per day.

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 Microfiltration is a membrane technical filtration process which removes contaminants
from a fluid (liquid and gas) by passage through a microporos membrane. A typical
microfiltration membrane pore size range is 0.1 to 10 micrometers (µm). Microfiltration is
fundamentally diffrenent from reverse osmosis and nanofiltration because those systems use a
pressure as a meaans 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.

AIM/OBJECTIVE

To study the characteristics of 4 different types of membrane silicon in terms of separation

process.

THEORY

The term membrane most commonly refers to a thin, film-like structure that separates

two fluids. It acts as a selective barrier, allowing some particles or chemicals to pass through,
but not others. In some cases, especially in anatomy, membrane may refer to a thin film that is
primarily a separating structure rather than a selective barrier.

A membrane is a selective barrier that permits the separation of certain species in a

fluid by combination of sieving and sorption diffusion mechanism. 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

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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 Figure 1.0 – process of membrane technology

The concept of a membrane has been known since the eighteenth century, but it
remained as only a tool for physical or chemical theories development until the end of World
War II, when drinking water supplies in Europe were compromised and membrane filters
were used to test for water safety. However, due to the lack of reliability, slow operation,
reduced selectivity and elevated costs, membranes were not widely exploited. The first use of
membranes on a large scale was with microfiltration and ultra-filtration technologies. Since
the 1980’s, these separation processes, along with electrodialysis, are employed in large plants
and, today, a number of experienced companies serve the market.

A membrane is a layer of material which serves as a selective barrier between

two phases and remains impermeable to specific particles, molecules, or substances when
exposed to the action of a driving force. 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). This

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separation process is purely physical and, thanks to its gentle separation, the use of both
fractions (permeate and retentate) is possible.

APPARATUS

1) Membrane Test Unit (Model TR14)

2) Digital Weighing Balance
3) Stopwatch
4) Beaker

MATERIAL
1) Sodium chloride.
2) Water.

PROCEDURE

General start-up procedure

1. All the valves were making sure initially closed.

2. A sodium chloride solution was prepared by adding 100g of sodium chloride into 20L
of water.
3. The tank was filled up with the salt solution that was prepared in step 2. The feed was
maintained at room temperature.
4. The power for control panel was turned on. All sensors and indicators were checked to
functioning properly.
5. Thermostat was switched on and the thermo oil level was checked to make sure it is
above the coil inside thermostat. The thermostat was checked if connections were
properly fitted.
The temperature was adjusted at the thermostat to maintain feed temperature.
6. The unit is now ready for experiments.

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Experiment procedure

1. The experiment was started with membrane 1. Valves V2, V5, V7, V11 and V15 were
opened.
2. To set the maximum working pressure at 20 bars, the plunger pump (P1) was switched
on and valve V5 was slowly closed. The pressure value at pressure gauge was
observed and the pressure regulator was adjusted to 20 bars.
3. Valve V5 was opened. Then, membrane maximum inlet pressure was set to 18 bars for
Membrane 1 by adjusting the retentive control valve (V15).
4. The system was allowed to run for 5 minutes. Sample from permeate sampling port
was collected and the sample was weighed using digital weighing balance. The weight
of permeates was recorded every 1 minute for 10 minutes.
5. The step 1 to 5 was repeated for Membrane 2, 3 and 4. The respective sets of valves
were opened and closed and the membrane maximum inlet pressure was adjusted for
every membrane.

Membrane Open Valves Sampling Retentive Membrane

Valves control valve maximum inlet
pressure(bar)

1 V2, V5, V7, Open V19 and V15 18

V11 and V15 close V11

2 V2, V5, V8, Open V20 and V16 12

V12 and V16 close valve V12

3 V2, V5, V9, Open V21 and V17 10

V13 and V17 close valve V13

4 V2, V5, V10, Open V22 and V18 8.5

V14 and V18 close V14

6. The graph of permeate weight versus time was plotted.

General shut-down operation

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 1. The plunger pump was switched off.
2. Valve 2 was then closed.
3. All liquid in the feed tank and product tank were drained by opening valves V3 and
V4.
4. The entire pipes were flushed with clean water. V3 and V4 were closed; the clean
water was filled to the feed tank until 90% full.
5. The system was run with the clean water until the feed tank is nearly empty.

RESULTS

Membrane 1

Times (mins) Weight of sample (g)

0 0
1 30.45
2 19.22
3 19.07
4 18.86
5 18.98
6 17.33
7 18.69
8 19.33
9 20.44
10 19.26

Membrane 2

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 Times (mins) Weight of sample (g)
0 0
1 75.23
2 64.24
3 59.23
4 69.88
5 66.03
6 66.25
7 64.50
8 67.39
9 64.81
10 67.80

Membrane 3

Times (mins) Weight of sample (g)

0 0
1 14.43
2 5.44
3 5.00
4 5.28
5 5.61
6 5.39
7 5.10
8 4.90
9 4.95
10 4.95

Membrane 4

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 Times (mins) Weight of sample (g)
0 0
1 112.30
2 127.38
3 128.16
4 133.84
5 147.35
6 145.02
7 146.77
8 146.51
9 144.23
10 145.71

DISCUSSION

This experiment has been done to fulfil the objective which is to perform a
characteristic study on four different types of membrane. 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.

In this unit, there are four types of membrane which each of them is differ with each
other. The four membranes I, II, III and IV are namely first, reverse osmosis (RO),
nanofiltration (NF), ultrafiltration (UF) and lastly microfiltration (MO) membranes
respectively while in the case of membrane type are AFC99, AFC40, CA202 and FTP100
respectively. Every type of this membrane has its own characteristics which differ in each
other as shown in table below;

Membran Material Max Max Max Apparent Hydro Solvent

e type pH pressur Temperatur Retention Philicit Resistanc
Rang e e character y e
e (bar) (℃ ¿

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 1 AFC99 Polyamid 1.5-12 64 80 99% NaCl 3 ++
e Film

2 AFC40 Polyamid 1.5- 60 60 60% CaCl 2 4 ++

e 9.5
Film

3 CA202 Cellulose 2-7.25 25 30 2000 MW 5 +

Acetate

4 FP100 PVDF 1.5-12 10 80 100,000M 1 +++

W

From the table above, its show that each membrane type have different characteristic
in each other. The first characteristics are based on its material. Membrane I and membrane II
were made up from the same element which is Polyamide Film while the other two
membranes were made up from cellulose acetate and PVDF. Polyamide film (membrane I and
II) is known as its permeability to water and its relative impermeability to various dissolved
impurities including salt ions and other small non-filterable molecules. Membrane III is made
of cellulose acetate which has an extremely low binding characteristic that made it ideal for
protein and enzyme filtrations. The material that membrane IV is made of is  polyvinylidene
difluoride (PVDF). PVDF is a material that can provide high protein and nucleic acid binding
capacity. In terms of maximum pH range, membrane I and IV have the maximum capacity of
range while membrane II and II were the least. While in properties of maximum operating
pressure, membrane IV shows the least operation while membrane I is the most maximum
operating unit in term of pressure.

The other characteristics of the membrane is apparent retention character with

membrane I rated as 99% NaCl rejection, membrane II with 60% CaCl 2 rejection, membrane
III with 2,000 MWCO and membrane IV with 100,000 MWCO. Furthermore, the membranes

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are characterized with their own hydrophilicity level. Hydrophilic membrane is a membrane
that has an attractive response to water and can readily adsorb water. This allows the material
to be wetted forming a water film or coating on the surface of the membrane. Hydrophobic
membrane is the opposite of it. Usually hydrophilic membrane has more charge than
hydrophobic membrane. Membrane III has the highest hydrophilic property followed by
membrane II, I and IV. These mean that membrane IV has the highest hydrophobic property
and usually known as hydrophobic membrane. In addition, membrane IV became the highest
solvent reistent other than the three membrane (I, II and III).

In doing this experiment, approximately about 100mL sodium chloride has been used
as the reagent (feed). The membrane has been set to a certain maximum pressure inlet for a
safety regulation so as not to exceed the maximum operation pressure of the membrane. Then,
the sample from permeate was collected for 10 minutes. In each 1 minute interval, the weight
of permeate was recorded. After the 10 minutes past, these steps were carried out again for the
others membranes unit. All the data got from this experiment was tabulated in the table in
result section. From the result, it shows the increasing in weight of permeate with time (as
time increase, weight of permeate increase) for all four membranes. Permeate is actually a
part of the feed stream that passed through the membrane, while a part of the feed that did not
pass through the membrane is called the retentate. In the graph plotted, it shows that there are
different permeation rate for each of membrane, with membrane IV has the highest
permeation rate followed by membrane II, I and lastly III. Thus, permeates moves faster
through membrane IV and slower in membrane III. The high permeation rate of membrane 4
is most probably due to its hydrophobic property, whereas the low permeation rate of
membrane 3 is most probably due to its hydrophilic property. The membrane separates a wide
range of particle sizes ranging from monoions to macromolecules.

In doing this experiment, the result get may be not 100% accurate although it follows
the theory. The error could be due to the lack of attention in doing the experiment, such as not
alert in taking the record in 1 minute’s interval and not accurate in adjusting the maximum
inlet pressure. This experiments can be improve by followed the recommendations suggested
at recommendation sections.

CONCLUSSIONS

As the conclusions, it can be said that the increase and decrease in the membrane were
almost similar to each other. Even though it was kind of hard to be detected, however, if the

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graph were properly analyzed, the curves for each and one of the membranes were almost the
same. However, the only things that distinguish these curves were the value plotted in each
curve. It can be seen based on the graph plotted; the value plotted for the first membrane was
the smallest. The value of the weight collected for each membrane increases along with the
membranes used. 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.

RECOMMENDATION

1) Repeat the experiment 2 or 3 times for each membrane in order to calculate the
average reading.
2) The digital weighing balance should not be put near the pump as it is moving while
taking reading. Thus error could be happen.
3) Wearing the gloves during taking the sample.
4) You must be alert with time during taking the sample.

REFERENCES

1) http://en.wikipedia.org/wiki/Membrane_technology

2) http://vedyadhara.ignou.ac.in/wiki/images/6/63/Unit_11_Membrane.DOC_1.pdf

3) http://www.epa.gov/ogwdw/disinfection/lt2/pdfs/guide_lt2_membranefiltration_final.
pdf

APPENDIX

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