Experiment 13 Ultrafiltration Unit

*Nurul Izian Binti Md Rejab, Christine Huan Sinwei, Teng Siaw Ping
Nuraini Nasuha Binti Mohd. Hami Nam
School of Chemical Engineering, Universiti Sains Malaysia, Seri Ampangan,
14300 Nibong Tebal, Penang, Malaysia.
*E-mail: yonz_sunkist@yahoo.com.my
Tel: 017-4352812

ABSTRACT

Ultrafiltration (UF) is a form of filtration that uses membranes to preferentially separate different
fluids or ions. Selectivity of membrane is based on molecular weight and size of the particles
contained in the solution. Suspended solids and solutes of high molecular weight are retained,
while water and low molecular weight solutes pass through the membrane. There are many
parameters that influence the removal of high molecular weight solids contained in juice: (a)
Operating Pressure-the flux is increase as the applied pressure increases; (b) Concentration of
solutes-in molecular filtration, the flow rate or flux is affected by concentration. As the
concentration of retained species increases, the flux will decrease; (c) % removal-Theoretically
the % removal will increase proportionally with the pressure.

1.0 Introduction

Ultrafiltration (UF) is a variety of membrane filtration in which hydrostatic pressure forces a

liquid against a semipermeable membrane. Suspended solids and solutes of high molecular
weight are retained, while water and low molecular weight solutes pass through the membrane.
This separation process is used in industry and research for purifying and concentrating
macromolecular (103 - 106 Da) solutions, especially protein solutions. Ultrafiltration is not
fundamentally different from reverse osmosis, microfiltration or nanofiltration, except in terms
of the size of the molecules it retains. Mostly, ultrafiltration is applied in cross-flow mode and
separation in ultrafiltration undergoes concentration polarization.

An ultrafiltration membrane is a membrane that effects separation on the principle of sieving.

The membrane has pores that are in the nanometre size range, and will therefore prevent
particles, colloids, microorganisms and dissolved solids that are larger in dimension than the
pores in the membrane surface from passing. The membrane therefore acts as a physical, size-
exclusion barrier, and it is for that reason that ultrafiltration membranes produce such a high
quality product.

Ultrafiltration’s main attraction is its ability to purify, separate, and concentrate target
macromolecules in continuous systems. Ultrafiltration does this by pressurizing the solution
flow. The solvent and other dissolved components that pass through the membrane are known as
permeate. The components that do not pass through are known as retentate. Depending on the
Molecular Weight Cut Off (MWCO) of the membrane used, macromolecules may be purified,
separated, or concentrated in either fraction.

The primary advantages of low-pressure UF membrane processes compared with conventional

clarification and disinfection (postchlorination) processes are:

 No need for chemicals (coagulants, flocculates, disinfectants, pH adjustment)

 Size-exclusion filtration as opposed to media depth filtration
 Good and constant quality of the treated water in terms of particle and microbial removal
 Process and plant compactness
 Simple automation.

Ultrafiltration (UF) is used to remove essentially all colloidal particles (0.01 to 1.0 microns) from
water and some of the largest dissolved contaminants. The pore size in a UF membrane is mainly
responsible for determining the type and size of contaminants removed. In general, membrane
pores range in size from 0.005 to 0.1 micron. UF membrane manufacturers classify each UF
product as having a specific molecular weight cutoff (MWC), which is a rough measurement of
the size of contaminants removed by a given UF membrane. A 100,000 MWC UF membrane
means that when water containing a given standard compound with a molecular weight of around
100,000 daltons is fed to the UF unit, nearly all of the compound will not pass through the
membrane.

Substances with a molecular weight of 100,000 daltons have a size of about 0.05 microns to
about 0.08 microns in diameter. UF membranes are used where essentially all colloidal particles
(including most pathogenic organisms) must be removed, but most of the dissolved solids may
pass through the membrane without causing problems downstream or in the finished water. UF
will remove most turbidity from water.

2.0 Materials and methods

 Figure 2.1: A view of the ultrafiltration unit

Figure 2.1 shows the apparatus used in this experiment. The schematic diagram of the
ultrafiltration unit is shown in the Figure 2.2. Basically the experiment consists of 2 parts:

PART A: Determination of membrane resistance, Rm

In this experiment, it is desired to find the resistance of membrane, R m by using de-ionized water.
Before the experiment starts, the unit operation that involves valve position and plunger pump is
checked and identified. Maximum pressure of 13.5 bar is set when running through the
ultrafiltration unit. The maximum pressure is set by first closing valves (V1) to (V5) and the tank
is filled with tap water. Then valve (V2) is opened and plunger pump is started. The pressure
gauge PG1 which is installed next to the pressure regulatory PR1 is observed. The pressure
regulator is adjusted to the desired maximum working pressure by using a wrench. The plunger
pump is stopped and valves (V2), (V4), (V5) and (V6) are reopened to drain off the water in the
tank. The feed tank is then filled with de-ionized water. All valves are checked and made sure in
the correct positions. The differential pressure is varied by adjusting the valve (V7), from 3 to 8
bar by increment of 0.5 bar. The permeate flux is calculated from the time of collection for 100
ml of permeate.

PART B: Ultrafiltration: Clarification of Orange Juice

A calibration curve of orange juice concentration vs. spectrophotometer readings (Absorbency,

Abs) as X and Y axis respectively is made by taking various concentration of juice which are 0.1,
0.2, 0.4, 0.6, 0.8, 1.0, 1.3, 1.4, 1.6, 1.8, and 2.0 (details of spectrophotometer can refer to
Appendix). Next, orange juice with concentration of 1% and 2% is prepared from de-ionized
water to make each solution of 20 liters in volume for experimental run of ultrafiltration unit.
Then the feed tank is filled with 20 liters of orange juice solution and is maintained at room
temperature. The maximum working pressure is set. All valves are checked and ensured to be in
the correct position. The plunger pump is started. Membrane inlet pressure is set to 3.0 bar by
adjusting valve (V7). The outlet flow rate is recorded from the flow meter. Similar with PART A,
the permeate flux is computed from the time of collection for 100 ml of permeate. The
concentration of orange juice in feed and permeate solution are determined from the
spectrophotometer reading and are recorded. The plunger pump was stopped and valve (2) is
closed. All the filtrate and retentate in the feed tank are mixed. These steps are repeated by
setting different inlet pressure from 4 to 7 bar with increment of 1.0.

Figure 2.2: Schematic diagram of ultrafiltration unit.

Equations employed when performing the experiment are as below:

Where Am = effective membrane area = 0.9 m2
t100 = time of collection for 100 ml of permeate
ΔV = volume of permeate collected = 100 ml

At the same time, according to Darcy’s equation,

Where ΔP = operating pressure / differential pressure (bar)

v = correction factor
Rm = membrane resistance (bar.s/cm)
Rc = cake resistance (bar.s/cm)

If fouling occurs within the membrane over time, the third resistance is introduced into the
equation:

Where Rf = resistance due to fouling

Initially the experiment is carried on by using pipe water. Since there are negligible large
molecular weight and size solutes in it, so no solute accumulate on the surface of membrane and
contribute no Rc. To compute the membrane resistance (Rm), we can assume that there is no
fouling effect occurs within the membrane. The flux equation is further reduced to

When flux (J) is plotted against ΔP,

So membrane resistance (Rm) can be determined.

For graph of % concentration of orange juice versus spectrophotometer reading (Absorbency,
Abs),

Since the graph is estimated to be a linear graph passing through the origin, the equation is
reduced to

Therefore % concentration of any feed stream (Cf) and permeate stream (Cp) can be calculated
based on the relation

Where Cf = % concentration of orange juice in feed stream

Cp = % concentration of orange juice in permeate stream
Absf = absorbency of feed stream
Absp = absorbency of permeate stream
The efficiency of ultrafiltration unit is determined by percent removal of solute from the feed
stream.
3.0 Result and discussion
Experiment A : Determination of Membrane Resistance, Rm
Table 1 Data for flux with varied differential pressures

Differential pressure, Permeate Flux, J

Volume,V (cm3) Time(s)
ΔP (kg/cm2) (cm/s)
3.0 100 133 0.0000835
3.5 100 100 0.0001111
4.0 100 71 0.0001565
4.5 100 64 0.0001736
5.0 100 55 0.0002020
5.5 100 45 0.0002469
6.0 100 39 0.0002849
6.5 100 34 0.0003268
7.0 100 29 0.0003831
Graph 1 Graph of flux versus Δ P

P
Permeate Flux is given as J 
 .Rm
From the plot of J versus ΔP, Slope = 1/ ν . Rm = 0.00004 m2.s / kg
Assume ν is a insignificant correction factor
Therefore, Membrane Resistance, Rm = 2.5 x 104 kg/m2.s

Experiment B : Clarification of Orange Juice

Table 2Calibration data for orange juice concentration vs spectrophotometer readings

Concentration ( % ) Spectrometer Reading

0.1 0.54
0.2 0.628
0.4 0.955
0.6 1.144
0.8 1.299
1.0 1.375
1.2 1.425
1.4 1.511
1.6 1.601
1.8 1.653
2.0 1.757

Graph 2 Calibration curve of orange juice concentration vs spectrophotometer readings

Table 3Data collected for 1% orange juice concentration

Differential Time (s) Permeate Permeated

Volume,V Average Spectrophotometer
pressure, ΔP Flux, J concentration % removal
(cm3) time (s) readings
(kg/cm2) (cm/s) (%)
1 2 3
3 100 114 119 121 118 0.099 0.0000942 0.0922647 90.7735322
4 100 71 70 76 72.33333 0.077 0.0001536 0.0717614 92.8238583
5 100 47 51 53 50.33333 0.078 0.0002208 0.0726934 92.7306617
6 100 36 36 37 36.33333 0.076 0.0003058 0.0708295 92.9170550
7 100 28 28 29 28.33333 0.082 0.0003922 0.0764212 92.3578751

Table 4Data collected for 2% orange juice concentration

Differential Time (s) Permeate Permeated

Volume,V Average Spectrophotometer
pressure, ΔP Flux, J concentration % removal
(cm3) time (s) readings
(kg/cm2) 1 2 3 (cm/s) (%)
3 100 132 141 136 136.33 0.083 0.00008150 0.00007595 99.99620226
4 100 90 88 93 90.33 0.092 0.00012300 0.00011463 99.99426835
5 100 65 64 66 65.00 0.060 0.00017094 0.00015931 99.99203447
6 100 48 50 45 47.67 0.006 0.00023310 0.00021724 99.98913792
7 100 42 40 41 41.00 0.010 0.00027100 0.00025257 99.98737173
Graph 3 Graph of flux versus operating pressure, ΔP

Graph 4 Graph of % removal versus operating pressure, ΔP

Discussion

Experiment A : Determination of Membrane Resistance, Rm

From graph 1, we observe that permeate flux is increasing proportionally with the operating
pressure. This fulfill the ultrafiltration equation

1 dV P P
J  
Am dt v Rm  Rc  V  Rm   Cb / Am  

The Rm value is a constant and can be obtained by the value of slope of the linearized graph
plotted.

Theoretically, membrane resistance, Rm is not a constant value as the resistance of membrane

increases with time progression. As time progresses, membrane will be clogged or filter cake
starts to build up.

Consequently, the membrane resistance, Rm increases as the increment of membrane resistance is

proportional to the increment of thickness of the filter cake. In addition, membrane resistance, Rm
also varies with differential pressure. This is because increasing of pressure drop will cause
higher liquid velocity. This will force additional particles of solid to go through the membrane
unit.

Experiment B : Clarification of Orange Juice

From graph 3 (graph of permeate flux versus operating pressure), we may conclude that the flux
is proportional to operating pressure. As pressure increase, flux will increase as well as in which
P
theoretically satisfy the equation J  . The permeate flux will increase with operating until
 .R m
it reaches a maximum steady state.

The feed with lower concentration has greater flux. It’s because the solution at higher
concentration contains more molecules and it will clog the membrane unit more easily, lowering
the flux. In general, we can say that the permeate flux for 1% concentration of orange juice is
always higher than the 2% concentration of orange juice at all values of operating pressure. The
1% concentration of orange juice is less concentrate and more dilute. Therefore solute can
manage to pass through the membrane. As for 2% concentration the solute is more concentrated,
this cause the solute more difficult to permeate through the membrane. As the concentration of
retained species increases, the flux will decrease.
From graph 4, % removal versus operating pressure shows that the % removal is almost constant
as the operating pressure increase. Theoretically the % removal will increase proportionally with
the pressure. The graph obtained may be due to membrane fouling and errors occurred when we
record the readings. The percentage of removal for 2% orange juice is higher. This is because the
more concentrated the solution, more molecules can be retained.

Concentration of Feed - Concentration of permeate

% Removal   100
Concentration of Feed

Error that may occur during experiment

 The membrane unit is contaminated before the experiment is being carried out. This is
because the membrane unit is saturated with juice, which is left after the previous group has
conducted the experiment. As a result, the absorbance value analyzed by the
spectrophotometer will be affected and thus, the permeate concentration and % removal are
inaccurate.
 The pressure cannot be maintained at steady state after reaching 5 bar. The indicator on the
pressure meter always vibrating and hence there is an parallax error when we taking the
readings.
 The volume of permeate samples collected is not consistent at high pressure due to the bad
performance of plunger pump which results in inconsistence of volumetric flow rate.

4.0 Conclusion

Rm is the intrinsic membrane resistance determined by using pure water as the feed. The value of
Rm we obtained from this experiment is 2.5 x 104 kg/m2.s.

From the ultrafiltration of orange juice process, we found that it’s important to choose the proper
membrane for the removal of particular molecules.

There are many parameters that influence the removal of high molecular weight solids contained
in juice: (a)Operating Pressure-the flux is increase as the applied pressure increases;
(b)Concentration of solutes-in molecular filtration, the flow rate or flux is affected by
concentration. As the concentration of retained species increases, the flux will decrease; (c) %
removal-Theoretically the % removal will increase proportionally with the pressure.

5.0 Acknowledgwment

The authors are grateful to the Universiti Sains Malaysia for providing experiment equipments
and materials needed in making the experiment successful. Special thanks to Dr. Sharif Hussein
Sharif Zein who is in-charge of the supervision of this experiment.

6.0 Nomenclature
Symbol Definition Unit
ΔP Differential pressure kg/cm2
V Volume cm3
T Time s
J Permeate flux cm/s
Rm Membrane resistance kg/m2.s

7.0 References

 McCabe, W.L., J.Smith and P.Harriott, “Unit Operations of Chemical Engineering”, 5 th

edition, McGraw Hill, 1993.

 Treybal, R.E, Mass Transfer Operations, Mc Graw Hill, USA, 1990.

 Third year chemical engineering laboratory manual.