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). The membranes tested are in different pressures. This membrane test unit
is a technology which fractionates materials through pores and minutes of gaps in the molecular
arrangement of continuous structure. We need to operate the plunger pump, control the valves, and
collect the samples as to weigh the samples. After the weighing of samples, 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 is used in reverse osmosis process and membrane 3 is in nanofiltration;
both of the tubes in the 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. This
experiment is conducted successfully.
INTRODUCTION

This 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, thus allowing
students or researchers to carry out membrane separation processes that are most widely used in the
food, dairy, pharmaceutical and chemical industries. 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 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.

The unit is suitable for carrying out a wide range of experiments such as:

 Dewatering
 Concentration
 Demineralisation
 Sugar removal
 Clarification

It is also possible to study the effect of varying the following process parameters on separation
performance:

 Flow rate
 Pressure
 Temperature

In this experiment we need to study the characteristic on the 4 different pressures of membranes. The
pressure is set at 4 different pressures for the membranes, which are:
 Membrane 1: 18 bar
 Membrane 2: 12 bar
 Membrane 3: 10 bar
 Membrane 4: 8.5 bar
AIMS

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).

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 N2from 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.
 Ranges of membrane based separations.

The selection of synthetic membranes for a targeted separation process is usually based on few
requirements. Membranes have to provide enough mass transfer area to process large amounts of feed
stream. The selected membrane has to have high selectivity properties for certain particles; it has to
resist fouling and to have high mechanical stability. It also needs to be reproducible and to have low
manufacturing costs. The main modeling equation for the dead-end filtration at constant pressure
drop is represented by Darcy’s law:
where Vp and Q are the volume of the permeate and its volumetric flow rate respectively (proportional
to same characteristics of the feed flow), μ is dynamic viscosity of permeating fluid, A is membrane area,
Rm and R are the respective resistances of membrane and growing deposit of the foulants. Rm can be
interpreted as a membrane resistance to the solvent (water) permeation. This resistance is a
membrane intrinsic property and expected to be fairly constant and independent of the driving force,
Δp. R is related to the type of membrane foulant, its concentration in the filtering solution, and the
nature of foulant-membrane interactions. Darcy’s law allows calculating the membrane area for a
targeted separation at given conditions. The solute sieving coefficient is defined by the equation:

where Cf and Cp are the solute concentrations in feed and permeate respectively. Hydraulic permeability
is defined as the inverse of resistance and is represented by the equation:

where J is the permeate flux which is the volumetric flow rate per unit of membrane area. The solute
sieving coefficient and hydraulic permeability allow the quick assessment of the synthetic membrane
performance.

There are two main flow configurations of membrane processes: cross-flow and dead-end filtrations. In
cross-flow filtration the feed flow is tangential to the surface of membrane, retentate is removed from
the same side further downstream, whereas the permeate flow is tracked on the other side. In dead-end
filtration the direction of the fluid flow is normal to the membrane surface. Both flow geometries offer
some advantages and disadvantages. The dead-end membranes are relatively easy to fabricate which
reduces the cost of the separation process. The dead-end membrane separation process is easy to
implement and the process is usually cheaper than cross-flow membrane filtration. The dead-end
filtration process is usually a batch-type process, where the filtering solution is loaded (or slowly fed)
into membrane device, which then allows passage of some particles subject to the driving force. The
main disadvantage of a dead end filtration is the extensive membrane fouling and concentration
polarization. The fouling is usually induced faster at the higher driving forces. Membrane fouling and
particle retention in a feed solution also builds up a concentration gradients and particle backflow
(concentration polarization). The tangential flow devices are more cost and labor intensive, but they are
less susceptible to fouling due to the sweeping effects and high shear rates of the passing flow. The
most commonly used synthetic membrane devices (modules) are flat plates, spiral wounds, and hollow
fibers.

Flat plates are usually constructed as circular thin flat membrane surfaces to be used in dead-end
geometry modules. Spiral wounds are constructed from similar flat membranes but in a form of a
“pocket” containing two membrane sheets separated by a highly porous support plate. Several such
pockets are then wound around a tube to create tangential flow geometry and to reduce membrane
fouling. Hollow fiber modules consist of an assembly of self-supporting fibers with a dense skin
separation layers, and more open matrix helping to withstand pressure gradients and maintain
structural integrity. The hollow fiber modules can contain up to 10,000 fibers ranging from 200 to 2500
μm in diameter; the main advantage of hollow fiber modules is very large surface area within an
enclosed volume, increasing the efficiency of the separation process.
APPARATUS

1. The Membrane Test Unit (TR14)

2. Sodium chloride solution

PROCEDURE

General start-up procedures

1. All valves were ensured to be initially closed.

2. A sodium chloride solution was prepared by adding 100 grams of sodium chloride into 20 litre of
water.
3. The tank was filled up with the salt solution prepared in step 2. The feed should always be
maintained at room temperature.
4. The power for the control panel was turned on. All the sensors and indicators were checked to
be functioning properly.
5. The thermostat was switched on and the thermo oil was made sure to be above the coil
thermostat. The thermostat connections were checked to be properly fitted.
6. The unit was ready for experiments.

General shut-down procedures

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

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

Procedures

1. The general start-up was performed.

 2. Valves V2, V5, V7, V11 and V15 were opened.
3. The plunger pump (P1) was switched on and valve V5 was slowly closed to set the maximum
working pressure at 20 bars. The pressure value at pressure gauge was observed and the
pressure regulator was adjusted to 20 bars.
4. Valve V5 was opened. 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 collected from permeate
sampling port and the sample was weighed using digital weighing balance. The weight of
permeates was recorded every 1 minutes for 10 minutes.
6. Step 1 to 5 for membrane 2, 3 and 4 were repeated. The respective valves were open and close
and membrane maximum inlet pressure was adjusted for every membrane.

Membrane Open valves (step 2) Sampling valves Retentate Membrane maximum

control valve inlet pressure(bar)

1 V2, V5, V7, V11, and Open V19 and V15 18

V15 closed V11

2 V2, V5, V8, V12 and Open V20 and V16 12

V16 closed V12

3 V2, V5, V9, V13 and Open V21 and V17 10

V17 closed V13

4 V2, V5, V10, V14 and Open V22 and V18 8.5
V18 closed V14

7. The graph of permeate versus time was plotted.

RESULTS

Time (min) Weight of permeates (g)

Membrane 1 Membrane 2 Membrane 3 Membrane 4
1 54.31 87.34 265.43 536.17
2 95.89 165.08 297.6 768.43
3 136.79 244.57 327.39 1001.07
4 178.67 321.65 357.81 1233.24
5 221.85 402.23 386.91 1465.07
6 262.37 482.05 418.09 1696.85
7 305.94 563.1 448.69 1924.43
8 348.37 642.37 479.79 2153.87
9 391.36 722.41 512.76 2393.55
10 434.61 808.71 539.92 2608.04

3000

2500
Weight of permeates (g)

2000
Membrane 1
1500
Membrane 2
1000 Membrane 3
Membrane 4
500

0
Time,t (min)
1 2 3 4 5 6 7 8 9 10

Graph of Weight of Permeates vs. Time

DISCUSSION
Membrane separation is based on separation mechanisms and size of the separated particles. The
membrane processes that have been widely used are microfiltration, ultrafiltration, nanofiltration,
reverse osmosis, electrolysis, dialysis, electrodialysis, gas separation, vapour permeation, pervaporation,
membrane distillation and membrane contactors. Pervaporation is the only process that involves phase
change. All processes except electrodialysis are pressure driven.
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). From
the graph that has been plotted, the slope of the membrane 4 is the steepest followed by membrane 2,
membrane 3 and membrane 1 respectively.
Based on the graph, membrane 1 is used for reverse osmosis process. This is because the weight of
permeates for membrane 1 has the lightest weight. Reverse osmosis operates at very high pressure
which is more than 20 bars. Reverse osmosis requires 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. Apart from that, nanofiltration is a
type of membrane process that uses membrane 3. It does not operate at the very high pressure as
reverse osmosis. The driving force used in nanofiltration is between 4 to 20 bars. Nanofiltration is used
for organic, color and contaminant removal as well as for softening. 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. Ultrafiltration operates at lower pressure compared to nanofiltration and reverse
osmosis. The driving force for this membrane is between 1-9 bars. Nanofiltration is applied in separation
of macromolecular solutions.
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 micrometers to pass through. The pressure used is basically 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.

CONCLUSION
From the experiment conducted, it can be concluded that membrane 1 is reverse osmosis, membrane 2
is ultrafiltration, membrane 3 is nanofiltration and membrane 4 is microfiltration. Membranes 1 and 3
operate at high pressure while membranes 2 and 4 operate at low pressure. This experiment is
performed successfully.
RECOMMENDATIONS
In this experiment, there are some recommendations that can be done in order to get the best results
which are:
 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.
 The average weight of permeates should be calculated by taking the weight of permeates in
three times in order to get more accurate value of weight of permeates.
 When collecting the sample from permeates sampling port, make sure that we used a big
container to support the volume of the sample and to avoid the sample from spill out in order to
get more accurate weight of permeates.
 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 of permeates.
 To collect the sample, the sampling valves should be open and close simultaneously so that
there is no interruption during collecting the sample from permeates sampling port.
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APPENDIX