UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

HEAT & MASS TRANSFER LABORATORY
(CHE504)

NAME : MUHAMMAD ILHAM HADI BIN HALIM

STUDENT NO. : 2017632206
GROUP : EH220 4H
EXPERIMENT : LAB 9- MEMBRANE SEPARATION
DATE PERFORMED : 23 MARCH 2018
SEMESTER :4
PROGRAMME / CODE : EH220
SUBMIT TO : MADAM SUFFIYANA AKHBAR

No. Title Allocated Marks (%) Marks

1 Abstract/Summary 5
2 Introduction 10
3 Aims 5
4 Theory 10
5 Apparatus 5
6 Methodology/Procedure 10
7 Results 10
8 Calculations 10
9 Discussion 20
10 Conclusion 5
11 Recommendations 5
12 Reference / Appendix 5
100
TOTAL MARKS

Remarks:

Checked by :

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Date :
1.0 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.
2.0 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

3.0 AIM

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).
4.0 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.MCLs are set as close to the health goals as possible after considering costs,
benefits, and the ability of public water systems to detect and remove contaminants using suitable
treatment technologies.
 Figure 1: 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.
5.0 APPARATUS

1. The Membrane Test Unit (TR14)

Figure 2: Membrane Test Unit (TR14)

2. Sodium chloride (NaCl) solution.

6.0 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 Sampling valves Retentate Membrane

2) control valve maximum inlet
pressure(bar)

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

and V15 closed V11

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

and V16 closed V12

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

and V17 closed V13

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

and V18 closed V14

7. The graph of permeate versus time was plotted.

7.0 RESULTS

Time (min) Weight of permeates (g)

Membrane 1 Membrane 2 Membrane 3 Membrane 4
1 20.35 56.91 15.33 74.85
2 28.07 110.21 19.84 131.53
3 35.25 142.30 23.97 191.78
4 44.27 168.94 27.98 251.64
5 52.32 250.00 32.37 309.68
6 60.12 294.18 36.21 369.77
7 68.27 340.54 40.11 430.69
8 75.98 387.90 43.59 491.57
9 83.50 432.35 47.14 549.36
10 89.87 479.80 50.52 608.90

Table 1: Data Collected

Figure 3: Graph of weight of permeates versus time

9.0 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 1 and membrane 3 respectively.

Based on the graph, we can see that the weight of permeates for membrane 3 has the lightest weight.
This is because membrane 3 is mainly used for reverse osmosis process. 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. Reverse osmosis also operates at very high pressure which is more than 20
bars. Only small amounts of very low molecular weight solute can pass through the membranes.

Other than that, an example of membrane process that used membrane 1 is nanofiltration. It does
not operate at the very high pressure as reverse osmosis. The driving force used in nanofiltration is
between 4 to 20 bars. Main application of nanofiltration is to separate small organic compounds
and multivalent ions. Nanofiltration is used for organic, colour and contaminant removal as well
as for softening. Nanofiltration is also applied in separation of amoxicillin from pharmaceutical
wastewater.

Next, Membrane 2 usually operates in ultrafiltration. Ultrafiltration was driven by a pressure

gradient, in which the membrane fractionates components of a liquid as a function of their solvated
size and structure. It also designates a membrane separation process. 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. Ultrafiltration can be used for the removal of particulates and macromolecules
from raw water to produce potable water.
The heaviest weight recorded is membrane 4. Membrane 4 usually used in microfiltration process.
In microfiltration, the membrane separation process is similar to ultrafiltration but it has larger size
of membrane pores. Thus, this will allow particles in the range of 0.1 to 10 micro meters 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.

Figure 4 : Characteristic of separation process

10.0 CONCLUSION

From the experiment that have been conducted, the results show that membrane 4 has the
heaviest weight of permeates (g) followed by membrane 2, membrane 1 and membrane 3. From
this result, we can identify which separation process is suitable for every membrane. As we can
see, membrane 4, which has the highest weight of permeates collected is mainly used in
microfiltration process. This is because membrane 4 it has the largest size of membrane pores
among those four membranes. The second highest is membrane 2. Membrane 2, is suitable to be
used in ultrafiltration because it has large membrane pores compare to membrane 1 and membrane
3. Next is membrane 1. This membrane usually used in nanofiltration process that usually operates
to remove contaminants. The driving force used in nanofiltration is between 4 to 20 bars. The last
is membrane 3. This membrane mainly used in reverse osmosis because it requires the greatest
operating pressure as it has the smallest pore-size range among those four membranes that suits
with membrane 3. So, we can conclude that every membrane have their own unique characteristics
and all membrane have their importance in various type of separation process.

11.0 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.
12.0 REFERENCES

1. (1986). Dairy Processing Handbook. In Dairy Processing Handbook (p. 125).

sweeden: Tetra Pak Processing Systems AB.
2. Eliane Rodrigues dos Santos Goes,Elisabete Scolin. Mendes, Nehemias Curvelo
Pereivela, Sueli Teresa Davantel de Barros. (2005). influence at different condition on
the concentration by reverse osmosis. Retrieved 9 april, 2012, from
Alim.Nutr.Araquara: http://serv-
bib.fcfar.unesp.br/seer/index.php/alimentos/article/viewFile/489/452
3. http://www.solution.com.my/pdf/TR14(A4).pdf. (n.d.). membrane test unit. Retrieved
9 april, 2012, from solteq: http://www.solution.com.my/pdf/TR14(A4).pdf
4. membrane separation technology primer. (n.d.). Retrieved 8 april, 2012, from asahi
kasei chemicals: http://www.asahi-kasei.co.jp/membrane/microza/en/kiso/index.html
5. nakagawa, o. (2012, february 12). membrane separation. Retrieved april 8, 2012, from
wikipedia:
http://en.wikipedia.org/wiki/Membrane_technology#Membrane_separation_processes
6. Ripperger S., Schulz G. (1986). Microporous membranes in biotechnical applications.
In Bioprocess Engineering (pp. 43-49).
7. Zeman, Leos J., Zydney, Andrew L. (Inc,1996). Microfiltration and Ultrafitration,
Principles and Applications. In M. Dekker, Microfiltration and Ultrafitration,
Principles and Applications. New York.
13.0 APPENDIX