ABSTRACT

This experiment is conducted to study the characteristics on 4 different types of membranes which are
AFC 99 (polyamide film), AFC 40 (polyamide film), CA 202 (cellulose acetate) and FP 100 (PVDF)
by using membrane test unit (TR14). Membrane separation is a technology, which fractionates materials
through pores and minutes of gaps in the molecular arrangement of a continuous structure. Membrane
separation can be classified by pore size and by the separation driving force for example Microfiltration
(MF), Ultrafiltration (UF), Nanofiltration (NF) and Reverse Osmosis (RO). We need to operate the
plunger pump, control the valves, and collect the samples as well as weighing the samples. After
weighing the sample, graph of permeates weight versus time is plotted.

Based on the graph, membrane 1 and membrane 3 used in membrane process that operates at higher
pressure while membrane 2 and membrane 4 used in membrane that operates at lower pressure.
Membrane 1 used in reverse osmosis process and membrane 3 is in Nanofiltration, which both of the
tubes in these membranes are fitted with polyamide. The tubes fitted in membrane 2 is
polyethersulphone which for ultrafiltration while for membrane 4 is PVDF which for microfiltration.
The membrane acts as a selective barrier allowing relatively free passage of one component while
retaining another. In membrane contactors, the membrane function is to provide an interface between
two phases but not to control the rate of passage of permeants across the membrane

The experiment was using approximately sodium chloride solution. 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 1517.46 g that is for membrane 4 and the lowest is about
881.32 g that is membrane 1. From the graph plotted, when the time increase the permeate weight also
increases. For the membrane 4, the line increases gradually while for the other 3 membranes the lines
show sloppier with increase in the percentage of composition of salt at product.
INTRODUCTION
Membrane is an interface that separates the two phases and restricts the transport of various chemical
species through it. Membrane can be homogeneous, heterogeneous, symmetric, asymmetric, charged
or neutral. In a membrane separation process, a feed consisting of a mixture of two or more components
is partially separate by means of a semipermeable barrier (the membrane) through which allow one or
more constituents of a mixture to pass through more readily than others and it involve in many
separation processes of gaseous or liquid mixture.

Semipermeable membranes, which usually are of thin layers of a rigid material such as porous glass or
sintered metal. However, in some cases, the membranes are purposely designed to be of flexible films,
which have high permeability types of molecules, and made from synthetic polymers. Nowadays, it is
important technical applications include drinking water by reverse osmosis (RO), filtrations in the food
industry, recovery of organic vapours and electrolysis for chlorine production.

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 design to demonstrate the technique of membrane separations
which has become highly popular as they provide effective separation without the use of the heating
energy in distillation process. Heat sensitive materials, such as fruit juices can be separated or
concentrated by virtue of their molecular weights. The unit consist of a test module supplied with four
different membranes, namely Reverse Osmosis (RO), Nano filtration (NF), and microfiltration (MF)
membranes.

This self-contained unit which coated by 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,
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 returned either 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 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 describes a process of water purification that remove contaminates 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 sulphate 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.

Microfiltration is a membrane technical filtration process, which removes contaminants from a fluid
(liquid and gas) by passage through a microporous membrane. A typical of microfiltration membrane
pore size range is 0.1 to 10 micrometres (µm). Microfiltration is fundamentally different from reverse
osmosis and Nano filtration 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

Figure 1: comparison between 4 type of membranes

The TR 14 unit is supplied with 4 membranes which are;

1. Membrane 1: AFC 99 (polyamide film)

2. Membrane 2: CA 202 (polyethersulphone)
3. Membrane 3: AFC 40 (polyamide film)
4. Membrane 4: FP 100 (PVDF)

The AFC 99 is rated with 99% NaCl rejection at maximum pressure and temperature which is 64 bar
and 80 ̊C whereas AFC 40 has 60% CaCl2 rejection at 60 bar and 60 ̊C. Both of these membranes use
in operation of reverse osmosis.

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 ̊C while
the FP 100 is at 10 bar and 80 ̊C
OBJECTIVES
 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. Its permits
the separation of certain species in a fluid by combination of sieving and sorption diffusion mechanism.
Separation is achieved by selectively passing 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, which
are 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 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.

Fiqure 2: process of membrane technology

Membrane separation can be classified by pore size and by the separation driving force for example
Microfiltration (MF),Ultrafiltration (UF), Nanofiltration (NF) and Reverse Osmosis (RO).

Figure 3: type of membrane used to separate components

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. When a hydraulic pressure is applied to the
concentrated solution, which is greater, and in reverse to the osmotic pressure, water molecules will
pass to dilute solution side through the membrane. This process can separate water from ions and low-
molecular weight organic constituents. Ultrafiltration enables precise separation, concentration and
purification of dissolved and suspended constituents based on the relative molecular size of substance.
Microfiltration membranes enable efficient and precise separation as well as concentration of suspended
and colloidal particles.

Figure 4: 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 -used for dehydration of whey, UF permeate and condensate.

 NF -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
.
APPARATUS
 Membrane Test Unit (Model TR14)
 Digital Weighing Balance
 Stopwatch
 Beaker

MATERIALS
 Sodium chloride
 Water

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. Make sure valve V2 is opened.
4. Valve V5 was opened. Then, membrane maximum inlet pressure was set to 18 bars for
Membrane 1 by adjusting the retentive control valve (V15).
5. 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.
6. V19 is opened and simultaneously V11 is closed to take the water sample.
7. 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 V12
3 V2, V5, V9, Open V21 and V17 10
V13 and V17 close V13
4 V2, V5, V10, Open V22 and V18 8.5
V14 and V18 close V14
General shut-down operation
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.

RESULT
time(min) Weight of permeates (g)
Membrane 1 Membrane 2 Membrane 3 Membrane 4
1 87.83 118.72 61.49 124.93
2 166.70 214.30 103.07 197.01
3 261.89 316.85 148.77 367.95
4 356.42 426.55 187.64 533.48
5 448.73 542.42 233.02 699.52
6 539.03 646.17 276.13 870.35
7 625.54 760.22 318.33 1045.96
8 713.64 870.01 375.19 1203.90
9 798.44 986.57 428.42 1361.61
10 881.32 1082.90 471.45 1517.46
Table 1: table of experimental result

Weight of permeates (g) vs time (min)

1600
weight of permeates (g)

1400
1200
1000
800
600
400
200
0
1 2 3 4 5 6 7 8 9 10
time (min)

Membrane 1 Membrane 2 Membrane 3 Membrane 4

Graph 1 : shows the correlation of weight of permeates (g) vs time (min)

DISCUSSION
We conduct this experiment to study the characteristics on 4 different types of membranes which are
AFC 99 (polyamide film), AFC 40 (polyamide film), CA 202 (cellulose acetate) and FP 100 (PVDF).
From the graph that has been plotted, the slope of the membrane 4 is the steepest compared to other
membranes. This followed by membrane 2, membrane 1 and membrane 3 respectively.

Membrane 1 and membrane 3 used in membrane process that operates at higher pressure while
membrane 2 and membrane 4 used in membrane that operates at lower pressure. Membrane 3 used in
reverse osmosis process and membrane 1 is in Nanofiltration, which both of the tubes in these
membranes are fitted with polyamide. The tubes fitted in membrane 2 is polyethersulphone which for
ultrafiltration while for membrane 4 is PVDF which for microfiltration.

Membrane 1 and 3 is shown as its permeability to water and its relative not permeability to various
dissolved impurities including salt ions and other small non-filterable molecules. Membrane 2 is made
of cellulose acetate, which has an extremely low binding characteristic that made it ideal for protein
and enzyme filtrations. The material used for membrane 4 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 2 and 4 have the maximum capacity of range while membrane 1 and
3 were the least. While in properties of maximum operating pressure, membrane 4 shows the least
operation while membrane 3 is the maximum operating unit in term of pressure.

Based on the result, the weight of permeates for membrane 3 have the lightest weight. Reverse osmosis
operates at very high pressure which is more than 20 bars. Reverse osmosis require the greatest
operating pressure as it has the smallest pore-size range and has the ability to remove solids as small as
salts. Only small amounts of very low molecular weight solute can pass through the membranes.
Membrane 3 is nonporous, asymmetric, and composite with homogeneous layer, which has dense pore
size. Reverse osmosis is mainly applied in production of pure water.

Apart from that, nanofiltration is also same as reverse osmosis that operates at high pressure but not as
higher as pressure used in reverse osmosis. The driving force used in nanofiltration is between 4 to 20
bars. Nanofiltration is used for organic, colour and contaminant removal as well as for softening.
Membrane 1 is also asymmetric, microporous, which has pore size between 1 to 5 nm. Main application
of nanofiltration is to separate small organic compounds and multivalent ions.

Membrane 2 operates in ultrafiltration. Ultrafiltration designates a membrane separation process, driven

by a pressure gradient, in which the membrane fractionates components of a liquid as a function of their
solvated size and structure. The membrane configuration is usually cross-flow. The feed water flows
across the membrane surface by limiting the extent of particle deposition and formation on the
membrane surface. The membrane pore size is larger allowing some components to pass through the
pores with the water. Ultrafiltration operates at lower pressure compared to nanofiltration and reverse
osmosis. This type of membrane is asymmetric microporous and the size of pore is 5-100nm. The
driving force for this membrane is between 1-9 bars

The membrane process for membrane 4 is microfiltration. In microfiltration, the membrane separation
process is similar to ultrafiltration but it has larger membrane pore size. Thus, this will allow particles
in the range of 0.1 to 10 micrometres to pass through. The pressure used is lower than that of
ultrafiltration process, which is 0.5 to 2 bars. The membrane configuration is usually cross-flow. This
membrane is symmetric and asymmetric porous. Microfiltration used in the clarification and sterile
filtration.
Furthermore, the membranes 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 3 has the highest hydrophilic property. These mean that membrane
4 has the highest hydrophobic property and usually known as hydrophobic membrane. In addition,
membrane 4 became the highest solvent resistant other than the three membranes.

The result of membrane 1, the weight of permeates after 10 minutes is 881.32g, and 1082.90g for
membrane 2, then it is 471.45g for membrane 3 which is the lowest and the highest weight of permeates
collected is from membrane 4 which is 1517.46g. 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 20 bar and membrane 4 is lowest with 2.3 bar. All the data got from this experiment
was tabulated in the table.

From the result, it shows that it is increasing in weight of permeate with time because as time increase,
weight of permeate also 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 4 has the highest permeation rate followed by membrane 2, 1 and lastly 3.
Thus, permeates moves faster through membrane 4 and slower in membrane 3. The other reasons to get
the result of permeates also depending to the flow rate of the system. If the flow rate is slower than the
solution, it 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 and size of pore in membrane can affect the amount
of permeate collected. If the size of pore is too small and the solution cannot pass through the pore and
amount of permeates also will less.
CONCLUSION
In this experiment, the equipment that been used is SOLTEQ membrane test unit (model; TR14). This
equipment was designed to allow the student to study the characteristics on 4 different types of
membrane based on the objective stated in this experiment. It can be concluded that the each membrane
have different types and different characteristic.

From the graph of membranes of permeate versus time shows that weight of permeate is directly
proportional to the time taken. The graph shown the slope of the membrane 4 is more sloped compared
to others membrane and it is the highest amount of permeate at product, which is 1517.46g. However,
the lowest is about 471.45g, which is the third membrane. This shows that every membrane will give
out the same pattern at the outlet but the values of the weight were different from each other. This is
due to the difference in pressure supply to the system and the size of pore depends on the type of
membrane used. Therefore, this shows that the separation process was the fastest in the fourth
membrane (microfiltration) and the third membrane (reverse osmosis) was the slowest.
RECOMMENDATION
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 shut8down
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 in order 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 and 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, each of membranes must be cleaned before and after usage to avoid fouling which might
affect the results. The amount of permeates should be recorded at the approximate moment to get the
accurate time. Furthermore, used the suitable size of jar based on the amount of permeate to prevent
spillage and affect the permeate weight of solution.
REFERENCE
 (https://www.sciencedirect.com/topics/earth-and-planetary-sciences/microfiltration, n.d.)
 (https://synderfiltration.com/learning-center/articles/membranes/membrane-processes/, n.d.)
 (http://www.thermopedia.com/content/948/, n.d.)
 (https://www.asahi-kasei.co.jp/membrane/microza/en/kiso/kiso_1.html, n.d.)
 (http://shodhganga.inflibnet.ac.in/bitstream/10603/156139/13/13_chapter%201.pdf, n.d.)
 (http://shodhganga.inflibnet.ac.in/bitstream/10603/156139/13/13_chapter%201.pdf, n.d.)