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UNIVERSITI TEKNOLOGI MARA

FACULTY OF CHEMICAL ENGINEERING


PROCESS ENGINEERING LABORATORY II
(CPE 554)

NAME
: AMIR FADZRUL BIN AB RAHMAN
STUDENT NO
: 2012289094
GROUP
: EH2214C (1)
EXPERIMENT
: MEMBRANE SEPARATION UNIT
DATE PERFORMED
: 16 APRIL 2013
SEMESTER
: MARCH- JULY 2013
PROGRAMME/ CODE : EH221
SUBMIT TO
: SITI SHAWALLIAH IDRIS

No.
1.

Title
Abstract/summary

Allocated marks (100%)


5

2.

Introduction

3.

Objectives/aims

4.

Theory

5.

Materials and apparatus

6.

Methodology/procedure

10

7.

Result

10

8.

Calculation

10

9.

Discussion

20

10. Conclusion

10

11. Recommendation

12. References

Marks

13. Appendix

Title

5 Page Number

AbstractMARKS
TOTAL

100

Introduction

Objectives

Theory

3-5

Apparatus

Methodology/Experimental Procedures

7-8

Results

Discussions

10-11

Conclusion

11

Recommendations

12

References

13

Appendices

13

Remarks:
Checked by:

Rechecked by:

..

Date:

CONTENT

ABSTRACT
The objective of this experiment is to study the characteristic of four different types of
membranes. 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). This experiment
requires approximately 100 gram of sodium chloride. The characteristics of the membranes
could be reverse osmosis, nanofiltration, ultrafiltration microfiltration membrane. 10 minutes
of time is required for every membrane in which the reading of the permeate is taken in every
1 minute. The data acquired were analysed and graphs of permeate weight versus time were
plotted. Based on the characteristics of every membrane and the results of the permeates, it
can be concluded that the type of membrane for membrane 1 is nanofiltration, membrane 2 is
ultrafiltration, membrane 3 is reverse osmosis and membrane 4 is microfiltration

INTRODUCTION
Separations by the use of membranes are playing an important role in the process
industries and biotechnology. In this relatively new separation process, 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 gases 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 this experiment, there are four types of membrane
separation process that are used. There are reverse osmosis, ultrafiltration, microfiltration and
nanofiltration membrane process.
Reverse osmosis is one of the types of membrane separation process. This membrane
separation process impedes the passage of low molecular weight solute which is placed
between a solute-solvent solution and a pure solvent. The solvent diffuses into the solution by
osmosis. In reverse osmosis, a reverse pressure difference is imposed which causes the flow
of solvent to reverse, as in the desalination of seawater. This process is also used to separate
other low molecular weight solutes, such as salts and sugars.
Other type of membrane separation process is ultrafiltration. This process use pressure
to obtain a separation of molecules by means of semipermeable polymeric membrane. The
membrane discriminates on the basis of molecular size, shape or chemical structures and
separates relatively high molecular weight solutes such as proteins, polymers and colloidal
materials. The osmotic pressure is usually negligible because of high molecular weights.
Microfiltration is also one of the membrane separation processes. In microfiltration,
pressure-driven flow through the membrane is used to separate micron-size particles from
fluid. The particles are usually larger than those in ultrafiltration. Examples are separation of
bacteria, paint pigment, yeast cells, and so on from solutions.

OBJECTIVES
The aim of this experiment is to study the characteristics on four different types of membrane
separation process for the removing of the solute from the solution.

THEORY
Numerous theoretical models for ultrafiltration, nanofiltration, and reverse osmosis
have been proposed along with the identification of new factor of controlling flux or mass
transfer through membranes. The basic operating patterns are best outlined in terms of the
hydrodynamic resistance resulting from the build-up of deposited materials on the membrane
surface. The flux, J will be given by
R
R
V C b
)]
Am
P
v ( m+ R c )=
1 dV P
J=
=

A m dt
v [ m+(

(1)

For most biological materials, is a variable depending on the applied pressure and time (the
compressible deposit), so that the expression requires a numerical solution. A useful method
for the effects of cross-flow removal of depositing materials is to write:

J=

P
v ( R m + Rd Rr )

(2)

Removal of solute by cross-flow is sometimes assumed constant, and equal to the convective
particle transport at steady state (J ssCb), which can be obtained experimentally or from an
appropriate model. In many situations however, steady state of filtration is seldom achieved.
In such cases, it is possible to describe the time dependence of filtration by introducing an

efficiency factor , representing the fraction of filtered material remaining deposit rather than
being swept along by the bulk flow. This gives:
Rc =

V C b
Am

, where 0 < < 1

(3)
Although deposition also occurs during ultrafiltration, an equally important factor
controlling flux is concentration polarization. Solution containing macromolecular gelforming solute will form a gel on the surface of the membrane. The gel formation will
contribute to formation of dynamics membranes.

Due to convective flux through the membrane a concentration of the solution at the
surface Cw increases and eventually reaches a gel formation concentration C g. The flux, J
through the membrane depends on a concentration according to the relationship:

J =k . ln

Cw
Cb

(4)
Combining equations (1) and (4),

ln

Cw
P
=
C b v ( Rm + R p ) k

(5)

As long as concentration Cw is less than Cg, Cw will increase with pressure, but the moment
Cw equals Cg, an increase in P brings about an increase of the layer resistance R p, and the
flux will no longer vary with pressure. Assuming no fouling effect, the membrane resistance
Rm can be calculated from the flux equation below:

J=

P
v Rm

(6)

The slope obtained from the plot of flux, J versus P is equal to

1
v R m . The retention of

any solute can be expressed by the rejection coefficient, R.


R=

ln (Cf /Co)
ln ( Vo/Vf )

(7)
where, Cf is final macrosolute concentration in the retentate
Co is initial macrosolute concentration
Vo is initial volume
Vf is final retentate volume
This expression assumes complete mixing of retentate seldom accomplished due to
concentration polarization. The apparent rejection coefficient depends on factors affecting
polarization including UF rate and mixing. For material entirely rejected, the rejection
coefficient is 1 (100%) rejection; for freely permeable material it is zero.
Rejection is a function of molecular size and shape. Nominal cut-off levels, defined
with model solute, are convenient indicators. Fractional rejection by membranes with low
MW cut-off spans a narrower range of molecular size than by more open membranes. For
maximum retention of a solute, select a membrane with nominal cut-off well below the MW
of the species.
Many biological macromolecules tend to aggregate so that effective size may be much
larger that native molecule, causing increased rejection. Degree of hydration, counter ions
and steric effects can cause molecules with similar molecular weights to exhibit very different
retention behaviour.

APPARATUS AND MATERIALS

TR 14 Membrane Test Unit apparatus.

500 mL beakers.

Electronic balance.

Sodium Chloride

Water

Figure 1:
TR

14
Membrane Test Units

PROCEDURE
OPERATING PROCEDURE
General start-up procedure
1. All the valves were ensured 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 prepared in step 2. The feed was
maintained at room temperature.
4. The power for control panel was turn on. All sensors and indicators were check to
functioning properly.
5. Thermostat was switch on and the thermo oil level was making sure above the coil
inside thermostat. 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.
General shut-down operation
1.
2.
3.
4.

The plunger pump was switch off.


Valve 2 was closed.
All liquid in the feed tank and product tank were drain by opening valves V3 and V4.
The entire pipes were flush 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 nearly empty for cleaning
purposed.
EXPERIMENT PROCEDURES
1. The general start-up procedures were performed.
2. The experiment for membrane 1 was start. Valves V2, V5, V7, V11, and V15 was
opened.
3. The plunger pump (P1) was switch on and slowly closed valve V5 to set the
maximum working pressure at 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. Sample was start to collect from
permeate sampling port and the sample was weight by using digital weighing
balanced. The weight of permeates was record every 1 minute for 10 minutes.
To collect sample, valve V19 was opened nad simultaneously closed valve V11.
6. The step 1 to 5 was repeated for membrane 2, 3, and 4. The valves was opened and
closed respectively and the inlet pressure in membrane was adjusted for every
membrane.
Membrane

Open

valves Sampling

(step 2)
V5,

valves

Retentate

Membrane

control valve

maximum inlet

V7, Open V19 and V15

pressure (bar)
18

V2,

V11 and V15


close V11
V2, V5, V8, Open V20 and V16

12

V12, and V16


close V12
V2, V5, V9, Open V21 and V17

10

V13, and V17


close V13
V2, V5, V10, Open V22 and V18

8.5

V14, and V18

close V14

7. The graph of permeates weight versus time was plotted.

RESULTS

Time (min)
1
2
3
4
5
6

Weight of permeates (g)


Membrane 1
Membrane 2
46.59
64.32
85.09
124.87
124.50
184.06
162.41
244.23
203.26
304.73
243.11
364.97

Membrane 3
40.31
71.41
103.98
135.38
167.51
199.57

Membrane 4
432.67
867.23
1294.82
1720.33
2146.62
2825.60

7
8
9
10

283.11
323.55
364.01
404.19

425.86
486.14
548.08
608.89

231.23
263.27
295.48
328.07

3247.61
3664.47
4082.05
4496.90

Permeates Weight versus Time


5000
4500
4000
3500
Membrane 1

3000

Permeates weight (g)

Membrane 2

2500

Membrane 3

2000

Membrane 4

1500
1000
500
0
0

10

12

Time (min)

DISCUSSIONS
The aim of this experiment is 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, we can observe that the slope of the
membrane 4 is the steepest compared to other membranes. This is followed by membrane 2,
membrane 1 and membrane 3 respectively.
Membrane 4 has the steepest slope compare to the other membranes. Therefore,
membrane 4 is the microfiltration. This is because the weight of permeates for membrane 4
have the heaviest weight. In microfiltration, the size of the membrane has large membrane
pore size. Thus, this will allow particles in the range of 0.1 to 10 micrometres to pass
through. The pressure used is basically in between 0.5 to 2 bars. The membrane configuration
is usually cross-flow. This membrane is symmetric and asymmetric porous.

While membrane 3 has the least steep slope compare to the other membranes.
Therefore, membrane 3 is the reverse osmosis. This is because the weight of permeates for
membrane 3 have the lightest weight. Reverse osmosis operates at very high pressure which
is more than 20 bras. 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.

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. A type of membrane 3 is asymmetric microporous and the size of pore is 5-100nm.
The driving force for this membrane is between 1-9 bars.

Nanofiltration is a type of membrane process that uses membrane 1. This 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, color and contaminant removal as well as for softening. Membrane 3 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.
CONCLUSIONS

From this experiment, it can be concluded that membrane 3 is operate in reverse osmosis
process while membrane 1 is in nanofiltration process. Both of this membrane process
operate at very high pressures and are typically deployed for the removal of dissolved
inorganic and organic constituents. While the membrane 2 and membrane 4 has been used in
ultrafitration and microfiltration respectively. Both of this membrane process are applied for
the removal of particulate and microbial contaminants and can be operated under negative or

positive pressure. The objective of this experiment is achieved and the type of the membrane
for all four membranes had been determined.

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.
The digital weighing balance should not be put near the pump as it is shaking while
taking reading. Thus, error could be happened.

REFERENCES

C.J Geankoplis, Transport Processes and Separation Process Principles, 4th edition
(Prentice Hall,2003)

http://www.solution.com.my/pdf/TR14(A4).pdf. (n.d.). membrane test unit. Retrieved


20 April, 2013, from solteq: http://www.solution.com.my/pdf/TR14(A4).pdf

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.

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

APPENDICES