EXPERI MENTAL MANUAL

MODEL: TR 14
SOLUTION ENGINEERING SDN. BHD.
NO.3, J ALAN TPK 2/4, TAMAN PERINDUSTRIAN KINRARA,
47100 PUCHONG, SELANGOR DARUL EHSAN, MALAYSIA.
TEL: 603-80758000 FAX: 603-80755784
E-MAIL: solution@solution.com.my
WEBSITE: www.solution.com.my
SOLTEQ

EQUIPMENT FOR ENGINEERING EDUCATION

054-0310-TR
MEMBRANE TEST
UNI T
MEMBRANE TEST
UNI T
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MEMBRANE TEST UNIT (Model: TR 14)_______________________________________________

Table of Contents


List of Figures . i

1.0 INTRODUCTION1

2.0 DESCRIPTION AND ASSEMBLY
2.1 Membrane and membrane housing 5
2.2 Pumps . 5
2.3 Tanks and Cooling/Heating System 6
2.4 Water Flow Meter .. 6

3.0 SUMMARY OF THEORY 7

4.0 OPERATING PROCEDURES
4.1 General Start-Up Procedures....11
4.2 General Shut-Down Procedures....11

5.0 EXPERIMENT PROCEDURES
5.1 Membrane Characteristic Study ....12

6.0 SAFETY PRECAUTIONS AND MAINTENANCE........13
6.1 Safety Precautions.13
6.2 Maintenance13

7.0 REFERENCES14

APPENDICES











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List of Figures

Page

Figure 1 Process Schematic Diagram 2

Figure 2 A classification of major types of membrane processes 3

Figure 3 A typical crossflow operation includes recirculation loop 4

Figure 4 Tubular (multichannel) type of microfilter 7

Figure 5 Concentration polarization at a membrane surface. Cw is the solute 9
concentration at the membrane surface and Cb is the bulk-solute
concentration

Figure 6 Typical dependence of membrane flux. 9


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1.0 INTRODUCTION
New chemical separation techniques such as membrane separations are becoming
increasingly popular as it provides effective separation without the use of heating energy as in
distillation processes. Heat sensitive materials can be separated or concentrated by virtue of
their molecular weights.
The Membrane Test Unit (Model: TR 14) is specially designed to allow students and
researchers to carry out the membrane processes that are widely used in biotechnology and
process industries the Reverse Osmosis (RO), Nanofiltration (NF), and Ultrafiltration (UF).
The process diagram is illustrated in Figure 1.
Ultrafiltration and microfiltration membranes are usually specified in terms of their "molecular
weight cut-off" (MWCO), whereas the nanofiltration and reverse osmosis membranes are
specified in terms of their percentage rejection of salts. Polymeric membranes are widely
used and supplied in the form of modules that give membrane areas in the range of 1 - 20 m
2
.
The membranes that are supplied with the model TR 14 unit is classified as tubular type
(Figure 2), which is widely used and have turbulent flow conditions. The system is in a cross
flow configuration where the feed solution is pumped parallel to the membrane at a velocity in
the range of 1 - 8 ms
-1

with a pressure difference of 0.1 - 0.5 MPa across the membrane. Liquid
permeates through the membrane and feed emerges in a more concentrated form on exit from
module.


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Figure1: Process Schematic Diagram
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Figure 2: A classification of major types of membrane processes






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The advantages of cross-flow membrane separations are

a) Higher overall liquid removal rate is achieved by preventing solid buildup on membrane surface.
b) The concentrate (retentate) remains in a mobile form suitable for further processing.
c) The solute content of the concentrate may be varied over a wide range.
d) It may be possible to fractionate solutes of different sizes.


CIRCULATION
SOLUTION TANK
CLEANING SOLUTION RETUM
FEED TANK
RECIRCULATION PUMP
SUSPENSION
RECIRCULATION
DRAIN/BLEED
CONCENTRATED
SUSPENSION
TI
PI
PI
FI
FI
PI
TI
FLOW INDICATOR
PRESSURE INDICATOR
TEMPERATURE INDICATOR
VALVE
FILTRATE
FEED
BANK OF CROSSFLOW FILTERS


Figure 3: A typical crossflow operation includes recirculation loop






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2.0 DESCRIPTION AND ASSEMBLY
2.1 Membrane and Membrane Housing

The P.C.I Single-tube Tester is designed for the economical, quick, initial evaluation of
membrane types and processes for separation and concentration at laboratory scale prior
to more detailed test work. It may be fitted with samples of any of PCIs wide range of
tubular reverse osmosis, nanofiltration and ultrafiltration membranes. Simply constructed in
316 stainless steel, the module has termination points allowing easy connection by flexible
or welded couplings to existing equipment.

The open channel, highly turbulent flow design allows a wide variety of process fluid to be
concentrated. It also allows simple clean-in-place techniques to be entirely effective.
The TR 14 unit is supplied with membrane:
i) Membrane 1: AFC 99 (Polyamide Film)
ii) Membrane 2: AFC40 (Polyamide Film)
iii) Membrane 3: CA 202 (Cellulose acetate)
iv) Membrane 4: FP 100 (PVDF)
The FP 100 PVDF membrane is rated with apparent retention character of 100000 MWCO
and CA 202 is 2000 MWCO. In addition, the AFC40 has 60% CaCl2 rejection and the
AFC99 is rated with 99% NaCl rejection.

2.2 Pump
2.2.1 CAT Triple Plunger Pump - Model 241

The CAT Triple Plunger pump is used to pump the liquid from the feed tank into the
membrane module.
Specifications:
Maximum flow rate : 13 liter/min.
Working pressure range : 7-85 bar
Max. fluid temperature : 71 C
Max. speed : 1725 RPM
Max. horsepower : 3.0 HP


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A CPC 7002 Pressure regulator is also installed to regulate the operating pressure of the
feed system.
Specifications:
Pressure regulated : 7-70 bar
Allowable flowrates : 3.8 - 38 liter/min.


2.3 Tanks and Cooling/Heating System
The TR 14 unit is supplied with a feed tank and a product tank, both having maximum
capacity of 15 liters. The feed and product tanks are made of stainless steel for corrosion
and chemical resistance. The retentate line is equipped with a unit of thermostat as heat
exchanger.

2.4 Water FlowMeter
The TR 14 unit is supplied with a Hedland turbine flow meter.






























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3.0 SUMMARY OF THEORY

Membrane separation technology has evolved from a small-scale laboratory technique to a large-
scale industrial process during the past 30 years. A classification of major types of membrane
processes is given in Figure 4. Numerous theoretical models for ultrafiltration, nanofiltration, and
reverse osmosis have been proposed along with the identification of new factors controlling flux or
mass transfer through membranes. The basic operating patterns are best outlined in terms of the
hydrodynamic resistance resulting from the buildup of deposited materials on the membrane
surface.



Figure 4: Tubular (multichannel) type of microfilter

The flux, J will be given by:

dt
dV
A
J
m
1
= =
( )
c m
R R v +

=
( ) [ ]
m b m
A VC R v / +

(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:
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( )
r d m
R R R v
J
+

= (2)

Removal of solute by cross-flow is sometimes assumed constant, and equal to the convective
particle transport at steady state (J ssCb
1 0 , < < =

Where
A
VC
R
m
b
c
), 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:
(3)
Although deposition also occurs during ultrafiltration, an equally important factor controlling flux is
concentration polarization. (Figure 5)
Figure 5. Concentration polarization at a membrane surface. Cw is the solute concentration at the membrane surface
and Cb, is the bulk-solute concentration.





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Typical operating patterns of ultrafiltration are shown in Figure 6c.

Figure 6. Typical dependence of membrane flux. (a) Applied pressure difference, (b) Solute concentration, (c)
Cross-flow velocity

Solution containing macromolecular gel-forming solute will form a gel on the surface of the
membrane. The gel formation will contribute to formation of dynamic membranes. The mechanism
is as follows:

Due to convective flux through the membrane a concentration of the solution at the surface Cw
increases and eventually reaches a gel formation concentration Cg
b
w
C
C
In k J . =
(Figure 6b). The flux, J through
the membrane depends on a concentration according to the relationship:

(4)

Combining Equations (1) and (4),

( )k C
C
In
b
w
p m
R R v
P

+

= (5)

As long as concentration Cw is less than Cg, Cw will increase with pressure, but the moment Cw
equals Cg , an increase in brings about an increase of the layer resistance Rp, and the flux will
no longer vary with pressure (Figure 7a).
Assuming no fouling effect, the membrane resistance Rm
m
R v
J
.

=
can be calculated from the flux equation
below:

(6)

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The slope obtained from the plot of flux, J versus is equal to
m
R v.
1


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


( )
f
f
V V n
C C n
R
/ 1
) / ( 1

0
0
= (7)
Where,
f
C is final macrosolute concentration in the retentate

0
C is initial macrosolute concentration

0
V is initial volume

f
V 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 3may be much larger that
the 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
behavior.
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4.0 OPERATING PROCEDURES

4.1 General Start-Up Procedures

1. Ensure all valves are initially closed.
2. Prepare a sodium chloride solution by adding 100 gram of sodium chloride into
20 liter of water.
3. Fill up the feed tank with the salt solution prepared in step 2. The feed shall
always be maintained at room temperature.
4. Turn on the power for the control panel. Check that all sensors and indicators
are functioning properly.
5. Switch on thermostat and make sure the thermo oil level is above the coil inside
thermostat. Check that thermostat connections are properly fitted.
Note: Adjust the temperature at the thermostat to maintain feed temperature.
6. The unit is now ready for experiments.


4.2 General Shut-Down Procedures

1. Switch off the plunger pump (P2).
2. Close valve V2.
3. Drain all liquid in the feed tank and product tank by opening valves V3 and V4.
4. Flush all the piping with clean water. Close V3 and V4, fill the clean water to
feed tank until 90% full.
5. Run the system with the clean water until the feed tank is nearly empty (this is
for cleaning purpose).
















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5.0 EXPERIMENT PROCEDURES

5.1 Membrane Characteristic Study
Objective:
In this experiment, students will perform a characteristic study on 4 different types
of membranes. This experiment requires approximately 100 gram of sodium
chloride.

Procedures:
1. Perform the general start-up procedures as described in Section 4.1.
2. Start the experiment for Membrane 1. Open valves V2, V5, V7, V11 and V15.
3. To set the maximum working pressure at 20 bars, switch on the plunger pump
(P1) and slowly close valve V5. Observe pressure value at pressure gauge
and adjust the pressure regulator to 20 bars.
Note: Use a proper wrench to turn the adjusting screw at the pressure
regulator (PR1) by turning clockwise to increase pressure and counter-
clockwise to reduce pressure.
Warning: Do not operate pump in dry condition. Make sure V2 is opened.
4. Open valve V5. Then, set membrane maximum inlet pressure to 18 bars for
Membrane 1 by adjusting the retentate control valve (V15).
5. Allow the system to run for 5 minutes. Start collecting sample from permeate
sampling port and weigh the sample using digital weighing balance. Record
the weight of permeates every 1 minute for 10 minutes.
Note: To collect sample, open valve V19 and simultaneously close valve V11.
6. Repeat the step 1 to 5 for Membrane 2, 3 and 4. Open and close the
respective sets of valves and adjust the membrane maximum inlet pressure
for every membrane.
Membrane
Open Valves
(Step 2)
Sampling
Valves
Retentate
control
valve
Membrane
maximuminlet
pressure (bar)
1
V2, V5, V7,
V11 and V15.
Open V19 and
close V11
V15 18
2
V2, V5, V8,
V12 and V16.
Open V20 and
close V12
V16 12
3
V2, V5, V9,
V13 and V17.
Open V21 and
close V13
V17 10
4
V2, V5, V10,
V14 and V18.
Open V22 and
close V14
V18 8.5

7. Plot the graph of permeate weight versus time.
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6.0 SAFETY PRECAUTION AND MAINTENANCE

6.1 Safety Precautions

1. Never operate the pump when there is no liquid in the pipeline. It will cause
serious damage to the pump.
2. High voltages exist and are accessible in the control panel. Return the unit to
your supplier for any servicing.
3. The system should not be subjected to shock, sudden impact, vibration,
additional load, or permanent external action of aggressive vapors.
4. Never splash water to the control panel. This will cause body injury and damage
to the equipment.
5. Never use your bare hand to test the AC Power Supply. It may cause hazardous
injury.
6. Leaking couplings or fittings should be carefully retightened. Replace any
gaskets or seals if necessary.


6.2 Maintenance

1. Always check and rectify any leak.
2. After each experiment, drain off any liquids from the feed tank and product
tank. Make sure that the feed tank, product tank and piping are cleaned
properly by flushing the system with water until no traces of chemical are
detected.
3. Dispose all liquids immediately after each experiment. Do not leave any
solution or waste in the tanks over a long period of time.
4. Wipe off any spillage from the unit immediately.
5. Check the lubricant oil level in the pump motor. Refill if the level is reduced
below the red spot










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7.0 REFERENCES

Warren L. McCabe, Julian C. Smith, Peter Harriott, Unit Operations of Chemical Engineering, 5
th

Edition, McGraw Hill, 1993

Christi J. Geankoplis, Transport Processes and Unit Operations, 3
rd
Edition, Prentice Hall
International Edition, 1995

Perry, R.H., Green, D.W. and Maloney, J.O., Perrys Chemical Engineering Handbook, 6
th
Edition,
McGraw Hill, 1984







































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APPENDICES


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APPENDIX A

SAMPLE TABLE FOR EXPERIMENT






















Time (min)
Weight of Permeates (g)
Membrane 1 Membrane 2 Membrane 3 Membrane 4
1

2

3

4

5

6

7

8

9

10

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APPENDIX B
SAMPLE EXPERIMENTAL RESULT








Time (min)
Weight of Permeates (g)
Membrane 1 Membrane 2 Membrane 3 Membrane 4
1 13.58 36.22 83.9 214.5
2 26.43 70.37 149.3 398.9
3 39.32 100.33 207.4 560.7
4 48.12 142.36 268.3 728.6
5 63.82 192.31 329.9 894.5
6 89.02 235.42 391.5 1058.9
7 117.62 280.17 459.1 1237.3
8 155.49 328.53 514.1 1381.8
9 229.29 376.81 575.4 1542.3
10 259.69 425.51 638.5 1704.1
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APPENDIX C