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International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 
E-ISSN: 2321-9637 
39 
Preparation, Characterization and Application of Ultra 
Filtration (UF) Membranes 
Rajesh Tripathy 
Department of Chemical Engineering, G H Patel College of Engineering & Technology, 
BakrolRoad,Vallabh Vidyanagar-388 120.Gujarat. India. 
Email: rajeshchemtech@gmail.com 
Abstract-In recent years, membranes and membrane separation techniques have grown from a simple laboratory 
tool to an industrial process with considerable technical and commercial impact. Today, membranes are used on a 
large scale to produce potable water from the sea by reverse osmosis, to clean industrial effluents and recover 
valuable constituents by electro dialysis to fractionate micro molecular solutions in the food and drug industry by 
ultra filtration, to remove urea and other toxins from blood stream by dialysis in an artificial kidney, to recover 
valuable products from waste like protein from waste whey and to release drugs such as scopolamine, nitroglycerine 
etc. at a predetermined rate in medical treatment.Although membrane processes may be very different in their mode 
of operation in the structures used as separating barriers. In many cases, membrane processes are faster, more 
efficient and more economical than conventional separation techniques such as distillation, extraction, adsorption, 
and absorption.[1,8] 
Index Terms-commercial impact, scopolamine, nitroglycerine, ultrafiltration 
1.0 INTRODUCTION 
Membranes have gained an important place in 
chemical technology and are used in a broad range of 
applications. The key property that is exploited is the 
ability of a membrane to control the permeation rate of 
a chemical species through the membrane. In 
controlled drug delivery, the goal is to moderate the 
permeation rate of a drug from a reservoir to the body. 
In separation applications, the goal is to allow one 
component of a mixture to permeate the membrane 
freely, while hindering permeation of other 
components. This paper provides a general 
introduction to membrane science and technology and 
cover Preparation, Characterization and Application of 
Ultra Filtration (UF) Membranes, that is topics that are 
basic to all membrane processes, such as transport 
mechanisms, membrane preparation, and boundary 
layer effects, cover the industrial membrane separation 
processes, which represent the heart of current 
membrane technology .Carrier facilitated transport is 
covered next, followed by reviewing the applications 
of membranes. The paper closes with that describes 
various minor or yet tobedeveloped membrane 
processes, including membrane reactors, membrane 
contactors for the separation of protein from different 
west, before disposal. 
1.1 Membrane Separation Processes 
All the membrane technologies are essential separation 
technologies depending upon size of the constitutes to 
be separated or on the ionic charges or absence of 
charges, diffusion into the matrix or some such 
transport phenomena. Keeping this in mind it is 
essential to mention here that none of the membrane 
technologies destroy the pollutants; they either separate 
or concentrate them for further easy handling. 
Membranes can be classified into 4 categories 
depending on the size of the materials they remove 
from the carrier liquid. The 4 categories, listed from 
the largest to the smallest pore size, are 
(a)Micro Filtration (MF) 
(b)Ultra Filtration (UF) 
(c)Nano Filtration (NF) 
(d)Reverse Osmosis (RO) 
a) Microfiltration (MF):MF is a low-pressure 
membrane process (0.3 to 3.3 bar) that removes 
particulate material ranging in size from 0.1 to 1.0 
microns (1,000 to 10,000 angstroms) and larger. MF is 
used for separating suspended or colloidal materials 
from a feed stream. Water, salts, and selected 
macromolecules pass through the semi-permeable 
membrane, and suspended solids are progressively 
concentrated. In the case of water, bacteria (like 
Escherichia coli, Cryptosporidium parvum, or Giardia 
lamblia) can be separated from water with this
International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 
E-ISSN: 2321-9637 
40 
technique. The salient features of the process are that it 
involves no phase change and it is relatively a low 
energy process. 
b) Ultrafiltration (UF):UF is a low-pressure membrane 
process (0.5 to 10 bars) that separates materials in the 
0.001 to 0.1 micron range (10 to 1,000 angstroms). UF 
is used for the separation of high molecular weight 
dissolved materials (solute). Water, salts, and low 
molecular weight species selectively pass through the 
semi-permeable membrane, and macromolecules and 
suspended solids are retained (progressively 
concentrated). UF separates bacteria and viruses from 
the water stream that MF passes because the pore size 
is smaller. 
c) NanoFiltration (NF):NF is a high-pressure 
membrane process used for separating materials less 
than 0.001 microns (10 angstroms) in size. NF is used 
for the separation of dissolved materials (solute). Less 
expensive, NF is not as fine a filtration as RO, but it 
also requires less energy to perform the separation (i.e. 
less operation & maintenance cost). In water, NF is 
very effective in removing hardness (multiple-charged 
ions), total dissolved solids, and natural organic 
material (Disinfection-By-Product DBP precursor 
material) with MF pre-filtration. NF is also known, in 
the water markets, as the "Membrane softening". 
d) Reverse osmosis (RO):RO membranes have the 
smallest pore structure, with pore diameter ranging 
from approximately 5-15 A0 (0.5 nm - 1.5 nm). The 
extremely small size of RO pores allows only the 
smallest organic molecules and unchanged solutes to 
pass through the semi-permeable membrane along with 
the water. Greater than 95-99% of inorganic salts and 
charged organics will also be rejected by the membrane 
due to charge repulsion established at the membrane 
surface. 
2.0 MATERIALS FOR MEMBRANE 
MANUFACTURING 
Pressure driven membrane separation processes fall 
into four broad categories: microfiltration, 
ultrafiltration, nanofiltration and reverse osmosis. The 
materials used for the preparation of these membranes, 
their morphological characteristics as well as their 
applications are different from each other. 
Morphologically the membranes are essentially porous 
in nature. Pore size in case of microfiltration 
membranes is in the order of 200 A0 (0.02 microns) to 
1,00,000 A0 (10 microns); in ultrafiltration the pore 
size is between of 20A0-200A0; in nanofiltration it is 
in the range of 10A0-20A0 and in the case of reverse 
osmosis it is between 1A0-10A0. Mechanisms of 
separation are also different for these membrane 
processes. While size based separations occur in case 
of microfiltration and ultrafiltration, membrane-solute 
interaction is the basis in nanofiltration and reverse 
osmosis. Application wise, microfiltration is used for 
the separation of solutes having molecular weight more 
than 3,00,000 Daltons, ultrafiltration is used for solutes 
in the range of 500-3,00,000 Daltons, nanofiltration is 
used for separation of solutes with a molecular weight 
range of 300-500 Daltons and reverse osmosis is used 
for the separation of solutes with molecular weight up 
to 300Dalton. Microfiltration is used for separation of 
suspended materials, coarse colloids, etc., 
ultrafiltration is useful in case of separation of soluble 
macromolecules, sugars, proteins, etc., nanofiltration is 
used in the separation of multivalent ions and reverse 
osmosis is used for the separation of ionic solutions. 
The membranes are predominantly polymeric in nature 
and is thin sheet like materials having typical thickness 
of the order of 100 microns. It forms a physical barrier 
between the fluids on either side, yet keeping 
communication between them. The crucial feature of a 
particular membrane is its selective permeability to 
certain species for which certain force is needed for the 
movement of species through the membrane. The 
overall driving force in the transport of species across 
the membrane is the chemical potential gradient, which 
is the sum of existing gradients such as concentration, 
pressure and electrical potential. In RO, water 
molecules are forced through the membrane by 
applying pressure. Material used for membranes are 
predominantly polymeric in nature. For RO, polymers 
such as cellulose acetate, polyamide, polyimide 
deposited on polysulphone base support etc. are used, 
whereas in ultrafiltration, the membrane used is made 
up of polysulfone and poly acrylonitrile.[7] 
2.1 Membrane Materials: 
These can be classified as (a) inorganic and (b) 
polymeric.
International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 
E-ISSN: 2321-9637 
41 
(a) Inorganic: Typical are gamma-alumina, alpha-alumina, 
borosilicate glass, pyrolyzed carbon, 
Zirconia/s. steel Zirconia/ carbon, etc. Other types of 
ceramic membranes are also being developed. 
Inorganic membranes have certain advantages over 
polymeric ones, like temperature and chemical 
stability. The cost of these materials and packing 
density (area /volume ratio) being the main restriction 
towards their large -scale applications. 
(b) Polymeric: typical materials, for Ultrafiltration are 
polysulphones, polyethersulphone cellulosic materials 
polyvinylidenefluoride, polyacrylonitrile, polyamides, 
etc the membranes are typically made by the phase 
inversion method. Behavior, performance, and 
limitations of some of the polymeric membrane are 
given below [1,2] 
1) Cellulose Acetate (CA) 
Raw material used is cellulose, which undergoes 
acetylation in presence of acetic anhydride, acetic acid 
and sulphuric acid. It is extensively used in UF studies 
as it is easy to fabricate less costly high salt retention 
and relatively high flux .The raw material cellulose is a 
renewable source. But it also has some drawbacks. 
Firstly it has fairly narrow range and maximum 
temperature recommended is 30 0C. This creates 
problems in maintaining sanitary condition and give 
lower flux .The PH range is also restricted between 2- 
8. Under acidic conditions polymer hydrolyses & 
structural integrity is lost. Under highly alkaline 
condition, deacetylation occurs, which will affect 
selectively, permeability. Also cellulose acetate has a 
poor resistance to chlorine .It also undergoes 
compaction and creep to a slightly greater extent 
pressure. Cellulose acetate is also biodegradable and 
hence storage properties. 
2) Aromatic polyamides (PA) 
It is also an important material for UF .It is 
characterized by the having an amide bond in its 
structure (--CONH--). In general they show good 
temperature resistance even up to 80 0C .The PH 
resistance is also good between range 3-11 at 25 0C 
.PA membranes are not biodegradable. Cleaning PA 
with acid caustic solutions is feasible but they are more 
sensitive to chlorine to CA and only polybenimidazole 
appears to show some resistance. 
3) Polysulfone (PS) 
PS is most widely used in UF. These membranes are 
characterized by having in its structure 
diphenylenesulfonerepeating units.It has wide 
temperature limits from 750C –1250C. Wide PH 
tolerance from 1-13. It has fairly good resistance and 
also it is not biodegradable. It is easy to fabricate 
membranes n wide variety of configurations and wide 
range of pore sizes. Cleaning using acids and bases and 
disinfections, using chlorine and H2O2 are feasible. PS 
is also resistant to strong oxidizing agent. Polysulfone 
has the apparent low-pressure limit. 
4) PAN (Polyacrylonitrile) 
PAN is hydrophilic in nature. It is not affected by 
boiling water .It is not affected by weak acids, weak 
alkalis but affected by strong acids & alkalis. It can be 
used up to 180 0C.Oxidising agent & common organic 
solvents have little effect. PAN membranes are hard, 
relatively insoluble & high melting material. 
5) Polyethersulfone (PES): 
PES is an amorphous material with a translucent amber 
tint. It has excellent dimensional stability and very 
good electrical insulation properties. It is also 
characterized by its creep resistance - substantial loads 
can be carried for long periods at temperatures up to 
180°C - and thermal stability PES parts can be used for 
thousands of hours up to 200°C with no significant loss 
of strength. It has relatively high water absorption and, 
in common with many other plastics, drying is 
essential before e.g. thermoforming. It has poor fatigue 
characteristics and is prone to environmental stress 
cracking but has good long-term thermal ageing 
resistance and reasonable radiation resistance. 
2.2 Selection Of Material 
It is evident that for selecting a membrane material 
which would be the best choice, it is necessary to 
consider operating condition like temperature, 
pressure; the nature of feed stream i.e. the pH, 
viscosity, density etc. and other factors like solid 
contents clean ability. 
Although the inorganic materials are having more 
temperature and pressure resistant, they can be used in 
very high or very low pH, we have chosen polymer 
membrane for casting and to study performance 
because polymer membranes are flexible in nature and 
can be casted in any shape but not the inorganic 
materials. Inorganic membranes are more tough cannot 
be casted easily.
International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 
E-ISSN: 2321-9637 
42 
There are many polymer membrane materials as 
discussed above but we have chosen polyethersulfone 
as a casting material because lot of study is done on 
other materials but polyethersulfone is not yet explored 
much as compared to other materials. 
Before going into details of the casting and 
performance study we will see some important 
physical and chemical properties of the 
polyethersulfone. 
Membrane materials characteristics 
a. The ideal membrane has the following 
characteristics: 
b. High water flux rates 
c. High salt rejection 
d. Tolerance to chlorine and other oxidants 
e. Resistance to biological attacks 
f. Resistance to Fouling by colloidal and 
suspended material 
g. Inexpensive 
h. Mechanical strength 
i. Chemical stability 
2.3 Membranes Used in present work : 
Polymeric 
- polysulfone/poly(ether 
sulfone)/sulfonatedpolysulfone 
- poly(vinylidene fluoride) 
- polyacrilonitrile 
- cellulosics 
- polyimide/poly(ether imide) 
- aliphatic polyamides 
- polyetheretherketone 
Ceramic 
- alumina (Al2O3) 
- zirconia (ZrO2) 
Solvent Used: 
-Dimethylformamide(DMF) 
-N, N-Dimethylacetamide.(DMAC) 
-Dimethylsulfoxide (DMSO) 
-N-Methylpyrrolidone(NMP) 
-Morfoline 
3.0Membrane Preparation Technique 
Anumber of different techniques are available to 
prepare synthetic membranes. Some of these 
techniques can be used to prepare organic (polymeric) 
as well as inorganic membranes. The most important 
techniques are: 
a. Sintering 
b. Stretching 
c. Track-etching 
d. Phase Inversion 
e. Coating 
Most commercially available membranes are obtained 
by phase inversion. This is a very versatile technique 
allowing all kind of morphologies to be obtained. This 
preparation technique is detailed as follows. Phase 
inversion is a process where a polymer is transformed 
in a controlled manner from a liquid to a solid state. 
The process of solidification is very often initiated by 
the transition from one liquid state in to two liquids 
(liquid0liquid demixing). At a certain stage during 
demixing one of the liquid phases (high polymer 
concentration phase) will solidify so that matrix is 
formed. By controlling the initial stage of phase 
transition the membrane morphology can be controlled, 
i.e., porous as well as nonporous membranes can be 
prepared. It covers different techniques like 
a. Solvent evaporation 
b. Precipitation by controlled evaporation 
c. Thermal precipitation 
d. Precipitation from the vapour phase 
e. Immersion precipitation 
The most commercially available membranes are 
prepared by immersion precipitation: a polymer 
solution (polymer + solvent) is cast on a suitable 
support and immersed in a coagulation bath containing 
a nonsolvent. Precipitation occurs because of the 
exchange of the solvent and nonsolvent. The 
membrane structure ultimately obtained results from 
the combination of mass transfer and phase separation.
International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 
E-ISSN: 2321-9637 
43 
3.1 Phase Inversion Process Of Membrane 
Manufacture: 
This refers to a method of manufacturing asymmetric 
membranes that result in a “solvent cast structure, 
which owes it porosity to immobilization of the 
polymer gel prior to complete solvent evaporation or 
depletion. This is accomplished by not allowing the 
cast solution to evaporate to dryness before its structure 
is set; partial solvent loss occurs so that the solution 
separates into two interspersed liquid phases. One of 
these phases represents the voids. As evaporation is 
allowed to continue, gel structure is set”. [1,8] 
The steps involved in preparation of Polysulfone 
membrane are, 
a. Preparation of polymer solution. 
b. Casting 
c. Gelation 
d. Annealing. 
Preparation of polymer solution 
The major constituents of Polysulfone membrane are 
classified into three types a) polymer base b) solvent 
and c) swelling agents (magnesium perchlorate or 
formamide). In addition few more chemicals may be 
added imparts certain properties of the membranes. 
Sometimes filler chemicals are also added with co-polymers 
to form better polymer chain links and 
improve mechanical strength. A clean, dry, glass 
beaker, washed with hydrochloric acid, is taken. It is 
then rinsed with acetone and kept to dry. The specific 
quantity of Polysulfone is poured into the beaker, 
which is followed by dimethylformamide. The stirring 
is stated at this point in order to get a homogeneous 
material. The remaining chemicals are then added 
slowly under continuous stirring using a glass stirrer. 
Proper care was taken to prevent the evaporation of 
solvents during the process. The polymerization was 
carried out for 4-5 hours. After this period, a viscous 
solution with lots of air bubbles trapped in it is 
obtained. The air bubbles trapped in it are removed by 
keeping the solution still for 3-4 hours. Thus a clear 
viscous solution is obtained 
Casting: 
The casting of Polysulfone membrane is done in a 
module. E.g. Flat sheet membranes are made by 
drawing the polymer solution over a glass plate using a 
“thin layer chromatography unit”. When this solution 
is cast and the solvent allowed to evaporate, it results 
in an increased concentration of polymer at the 
solution/ air interface, since solvent is lost more rapidly 
from the surface. The polymer essentially goes out of 
solution at the surface and forms the so-called skin 
layer that is characteristic of asymmetric membranes. 
(This phenomenon is analogues to “case hardening” in 
products that have been rapidly dried.). After the skin 
forms, the remaining solvent in the bulk of the mixture 
evaporates more slowly. Eventually the swelling agent 
in the mixture starts separating out as a different phase, 
resulting in two phases within the substructure: the 
polymer solvent as the concentrated phase and the 
swelling agent as the dispersed phase. 
Gelation: 
The polymer film this formed is further consolidated 
by a process of gelation. Here, the polymer chain is 
uniformly linked and distributed in the proper 
orientation for flow of permeate. Gelation is obtained 
by keeping the membrane in water at a low 
temperature of about 5-6 oC. 
Annealing: 
The polymer film thus produced, having a hard crust 
layer on spongy porous support, is still mechanically 
weak and highly compressible. With application of 
pressure the pores can be easily stretched. These are 
hardened with consequent shrinkage of pores by means 
of proper heat treatment of the membrane. This can be 
achieved by the process of annealing.The peeled sheet 
is immersed in hot water for a period of five minutes; 
the membrane is maintained at 70oC. Product flux and 
solute rejection can be controlled buy a process 
condition of this step. Higher temperature causes a 
decrease in flux of product water and an improvement 
in solute rejection and vise –versa. Since the degree of 
rejection can be adjusted by changing the heating 
temperature, this step is very important in membrane 
preparations. 
3.0 RESULTS AND DISCUSSION 
3.1 Analysis of Protein Solution 
To study the performance of ultrafiltration membrane 
experimentation is done on dairy whey /milk/protein 
solution .In this report, to study the performance of PS 
membrane which are casted in laboratory, the standard 
protein solution is used. The concentration of BSA 
protein solution used for experimentation is 0.5%.
International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 
E-ISSN: 2321-9637 
44 
0.4 
0.35 
0.3 
0.25 
0.2 
0.15 
0.1 
0.05 
0 
0 0.2 0.4 0.6 
Absorbance 
protein conc. (%) 
Series2 
Linear 
(Series2) 
First of all protein solution is prepared, then by biuret 
method calibration chart is plotted. Then this 
calibration chart is used for determination of 
concentration of permeate. The standard protein 
solution is prepared as follows, 
1. Preparation of standard BSA solution 
Take 50 mg of BSA protein powder in conical flask 
and dilute it in 10 ml of distilled water. Then the 
standard protein solution i.e. the solution having 0.5 % 
concentration will be ready for membrane 
characterization. First of all by using this BSA solution 
one can plot a calibration curve, which will be helpful 
for the analysis of permeate obtained stirred cell 
apparatus. 
3.2. Analysis of BSA by Biuret Method 
a) Preparation of biuret reagent: 
Dissolve 9 gms. of sodium potassium tartarate in 
approximately 400 ml of 0.2 N NaOH. Dissolve 
separately 3 gm of CuSO4.H2O in minimum quantity of 
distilled water & transfer slowly with constant stirring 
to sodium potassium tartarate. Then add 5 gm of 
potassium iodide & adjust the whole solution to 1000 
ml by addition of 0.2 N NaOH. 
b) Preparation of calibration chart: 
Six test tubes were taken. A sample of BSA solution of 
0.5% concentration and water were prepared in six test 
tubes according to the table given. And four ml of 
biuret reagent was added in each test tube. Incubate 
this solution at room temperature for ½ an hour and 
absorbance was measured at 530 nm for the respective 
samples in spectrophotometer. The respective 
absorbance with different concentration of protein 
solution is shown in table 5.1. Now the absorbance at 
the respective concentration is known so the calibration 
curve between absorbance and protein concentration is 
drawn as shown in figure 1. 
Table .1 Calibration chart. 
Std 
.BS 
A 
ml 
Distille 
d 
water 
ml 
Biuret 
Reage 
nt 
ml 
Protein 
concentrati 
on (wt/vol) 
% 
Absorban 
ce 
At 530 nm 
0.0 1.0 4 0.0 -- 
0.2 0.8 4 0.1 0.094 
0.4 0.6 4 0.2 0.2 
0.6 0.4 4 0.3 0.217 
0.8 0.2 4 0.4 0.283 
1.0 0.0 4 0.5 0.333 
Figure 1. Calibration Curve 
From this calibration curve concentration of permeate 
(less than 0.5% concentration) can be obtained. This 
calibration curve has a limitation that conc. more than 
0.5% can not be taken in a feed as the curve shows 
straight line nature up to 0.5% concentration. 
3.3 Stirred cell Apparatus 
Construction: 
The stirred cell apparatus consist of [1] 
a. Cell cylinder 
b. Pressure gauge 
c. Compressor 
d. Magnetic stirrer 
A] Cell cylinder: It consists of 
a. Pressure inlet: For applying pressure to feed. 
b. Pressure release valve: To release pressure in 
the cell cylinder. 
c. Transparent acrylic body. 
d. O – ring: To fit the membrane on membrane 
support. 
e. Stirring bar: For stirring of solution. 
f. Membrane 
g. Membrane support: To fit the membrane in 
cell cylinder. 
h. Filtrate out: To collect the permeate. 
B] Pressure gauge: It is used to apply the pressure 
inside the cell. 
C] Compressor: Compressed air is sent at 1 – 2 kg/cm2 
in cell cylinder. 
D] Magnetic stirrer: Cell cylinder is mounted on 
magnetic stirrer which in tern is used to stir the stirring 
bar placed inside the cell cylinder.
International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 
E-ISSN: 2321-9637 
45 
Figure 2. (a) Stirred cell Apparatus schematic diagram 
Figure 2.(B)Working model of Stirred cell 
ApparatuswithUltrafiltration of BSA Protein solutions. 
Working: 
Part A: Measurement of Distilled water flux. 
Take 50-60 ml of distilled water in stirred cell. Start 
magnetic stirrer. Maintain moderate rpm. Start Air 
compressor and maintain the pressure on the pressure 
gauge as 1 Kg/Cm2 .As soon as the pressure is 
developed, start the stopwatch. Note down Time 
required to collect 1 ml of permeate. Take 30-40 
readings. 
Part B: Measurement of BSA Protein solution flux/ 
milk flux/Whey Flux. 
Take 50-60 ml of known concentration of protein 
solution/whey/milk as feed solution in stirred cell. Start 
magnetic stirrer. Maintain moderate rpm. Start Air 
compressor and maintain the pressure on the pressure 
gauge as 1 Kg/Cm2 .As soon as the pressure is 
developed, start the stopwatch. Note down Time 
required to collect 1 ml of permeate. Take 30-40 
readings. 
Part C: Measurement of volume concentration factor. 
The stirred cell experiment as mentioned in 
measurement of BSA protein solution flux was 
performed. After 5 minutes amount of permeate 
collected was noted and after each 4 ml time required 
was noted. 3-4 readings were taken. 
VCF is calculated by,VCF= volume of feed / volume 
of rententate 
Part D: Measurement of Rejection 
The standard stirred cell experiment for BSA protein 
solution was performed and after 4 ml time required to 
collect permeate was noted and flux is calculated. The 
absorbance of each 4ml permeate was noted and 
overall absorbance was noted. Permeate concentration 
was calculated from the calibration curve. 
The Rejection is calculated by R = 1-Cp / Cf 
Where,Cp: Concentration of permeate in % wt / vol 
Cf: Concentration of feed in % wt / vol 
4.0 MEMBRANE CHARACTERIZATION 
1. Thickness: 
The thickness of standard UF membrane ranges from 
20 – 100 micron. The thickness of casted membrane is 
measured with the help of micrometer screw gauge at 
different points on the membrane and the average 
thickness is calculated. It is used in the measurement of 
pore diameter and porosity. 
2. Porosity: 
Porosity is the ratio of pore volume of the membrane to 
the total volume of membrane. 
It is calculated as follows, 
1. Take wt. of wet membrane (in water). 
2. Dry the membrane in oven for few minutes & take 
its dry weight. 
3. Take the difference & multiply with density of water 
that will give you the pore volume of membrane. 
4. From area & thickness of membrane calculate 
volume of membrane.
International Journal of Research in Advent Technology, Vol.2, No. 
5. Ratio of pore volume to membrane volume will give 
you porosity. 
Porosity = pore volume/ membrane volume 
5 .0 MATERIALS AND METHODS 
5.1. Materials 
Polysulfone (PS) in powder form was obtained from 
M/s. Gharda Chemicals Company, India. The solvents 
used for membrane making are N,N 
formamide (DMF) and were of reagent grade. 
Polyethylene glycol (PEG), Polyvinyl Pyrrolidone 
(PVP K-30) of different molecular weights and 
piperazine (AR grade) were locally procured and used 
as additives. 
5.2. Preparation of membrane 
In airtight glass bottle, a specified quantity of polymer 
was taken and then a known quantity of 
the solvent was added. The solution w 
for several hours for complete dissolution.Calculated 
quantities of additives were subsequently added and 
the solution was homogenizedand kept for deairation. 
The solution viscosity was measured using a standard 
Brookfield viscometer.The dope solution thus obtained 
was spread over a smooth glass plate with the help of a 
knife edge. The thickness of the membranes was 
controlled by varying the thickness of adhesive tapes at 
the sides of the glass plate. The glass plate was kept in 
an environment of controlled temperature and humidity 
during membrane casting. No deliberate solvent 
vaporation period was allowed. The glass plate was 
subsequently immersed in a gelling bath, which is 
generally demineralized water maintained at a known 
temperature otherwise as mentioned in the 
text.Immediately phase inversion starts and after 
fewminutes thin polymeric film separated out from the 
glass. It was repeatedly washed with demineralized 
water and wet stored. The actual thickness of the 
membranes was measured using a micrometer. 
Table 2. Dope solution compositions 
Dop 
e PS 
Compositio 
n in Wt. % 
PS 
Solutio 
n DMF 
Additiv 
M 1 16 84.9 
M 2 16 80.6 
M 3 16 74.3 
E-ISSN: 2321-9637 
N-dimethyl 
nt was kept agitated 
ope ent therwise e 1 
Wt. % 
Additiv 
e 2 
Wt. % 
0 3.5 
4 3.5 
10 3.5 
Sl No Volume 
DW 1 ml 
M 1.1 
BSA 1 0-5 
BSA 2 05--10 
BSA 3 10--15 
BSA 4 15-20 
M 1.2 
P Whey1 0-5 
P Whey2 05--10 
P Whey3 10--15 
P Whey4 15-20 
Results of M-1 
in ml 
Time in 
Sec 
Table 3.Effect of the time on the 
Membrane Flux 
Figure 3.Effect of the time on the performance of 
Membrane Flux 
Figure 4.Effect of the time on the performance of 
Membrane Flux 
3, March 2014 
46 
performance of 
model M 1.1 
model M 1.2 
Flux 
lt/hr.m2 
190 20.105 
212 18.019 
267 14.307 
295 12.94 
308 12.4 
493 7.74 
520 7.34 
551 6.93 
606 6.303
International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 
E-ISSN: 2321-9637 
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Table 4. Effect of the Pressure on the performance of 
Membrane Flux 
Sl No 
Pressure 
kg/cm2 
Time in 
Sec 
Flux 
lt/hr.m2 
M1.3 
DW 1 0.50 306 12.48 
DW 2 1.00 190 20.1 
DW 3 1.20 180 21.22 
DW 4 1.40 163 23.43 
M1.4 
BSA 1 0.50 277 13.79 
BSA 2 1.00 213 17.93 
BSA 3 1.20 185 20.64 
BSA 4 1.40 160 23.87 
25 
20 
15 
10 
5 
Figure 5.Effect of the Pressure on the performance of 
Membrane Flux M 1.3 
30 
25 
20 
15 
10 
5 
Figure 6.Effect of the Pressure on the performance of 
Membrane Flux M 1.4 
Results of M-2 
Table 5.Effect of the time on the performance of 
Membrane Flux 
Sl No 
Volume in 
ml 
Time in 
Sec 
Flux 
lt/hr.m2 
DW 1 ml 19 201.05 
M 2.1 
BSA 1 0-5 52 73.46 
BSA 2 05--10 70 54.57 
BSA 3 10--15 90 42.44 
BSA 4 15-20 103 37.08 
M 2.2 
P Whey1 0-5 109 35.046 
P Whey2 05--10 151 25.29 
P Whey3 10--15 163 23.43 
P Whey4 15-20 174 21.95 
80 
70 
60 
50 
40 
30 
20 
10 
Figure 7..Effect of the time on the performance of 
Membrane Flux M 2.1 
40 
35 
30 
25 
20 
15 
10 
5 
Figure 8.Effect of the time on the performance of 
Membrane Flux M 2.2 
M 1.3 
0 
0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 
Pressure in Kg/cm2 
F lu x 
M 1.4 
0 
0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 
Pressure in Kg/cm2 
F lu x 
M 2.2 
0 
0 20 40 60 80 100 120 140 160 180 200 
Time in Sec 
F lu x 
M 2.1 
0 
0 20 40 60 80 100 120 
Time in Sec 
Flux
International Journal of Research in Advent Technology, Vol.2, No. 
Table 6.Effect of the Pressure on the performance of 
Membrane Flux 
Figure 9. Effect of the Pressure on the performance of 
Membrane Flux M 2.3 
Figure 10.Effect of the Pressure on the performance of 
Membrane Flux M 2.4 
Sl No 
Pressure 
kg/cm2 
Time 
in Sec 
M 2.3 
DW 1 0.50 33 
DW 2 1.00 19 
DW 3 1.20 16 
DW 4 1.40 12 
M 2.4 
BSA 1 0.50 148 
BSA 2 1.00 58 
BSA 3 1.20 52 
BSA 4 1.40 50 
E-ISSN: 2321-9637 
Results of M-3 
Table 7. Effect of the time on the performance of 
Membrane Flux 
Sl No 
Volume 
in ml 
DW 1 ml 
M 3.1 
BSA 1 0-5 
BSA 2 05--10 
BSA 3 10--15 
BSA 4 15-20 
M 3.2 
P Whey1 0-5 
P Whey2 05--10 
P Whey3 10--15 
P Whey4 15-20 
Figure 11. Effect of the time on the performance of 
Membrane Flux M 3.1 
Figure 12. Effect of the time on the performance of 
Membrane Flux M 3.2 
Flux 
lt/hr.m2 
115.75 
201.05 
238.75 
318.33 
25.81 
65.85 
73.462 
76.4 
3, March 2014 
48 
Time 
in Sec 
Flux 
lt/hr.m2 
26 146.92 
90 42.44 
144 26.52 
160 23.87 
179 21.34 
192 19.89 
230 16.6 
283 13.49 
310 12.32 
.
International Journal of Research in Advent Technology, Vol.2, No. 
Results of M-3 
Table 8.Effect of the Pressure on the performance of 
Membrane Flux 
Sl No 
Pressure 
kg/cm2 
Time 
in 
Sec 
M 3.3 
DW 1 0.50 38 
DW 2 1.00 26 
DW 3 1.20 20 
DW 4 1.40 18 
M 3.4 
BSA 1 0.50 87 
BSA 2 1.00 75 
BSA 3 1.20 64 
BSA 4 1.40 60 
Figure 13.Effect of the Pressure on the 
Membrane Flux M 3.3 
E-ISSN: 2321-9637 
Flux 
lt/hr.m2 
100.52 
146.92 
191 
212.22 
43.9 
50.93 
59.93 
63.66 
performance of 
3, March 2014 
Figure 14.Effect of the Pressure on the performance of 
Membrane Flux M 3.4 
6.0 CONCLUSION AND FUTURE SCOPE 
Aseries ofUtrafiltration PS membrane was successfully 
casted & performance was studied for M– M 
1,M– 2 and 
M – 3 (distinction based on polymer concentration and 
additive concentration and the effect with different 
solvents).Stirred cell operation was performed with 
standard Bovoin Serum Albumin (BSA) protein 
solution (0.1 % concentration).,Distilled water flux, 
Dairy Waste with different pressure range starting from 
0.5-1.4 kg /cm2.We have observed that for three 
membranes as the time increases flux goes on 
decreases due to fouling.Rejection increases with 
increase in PS concentration in ultrafiltration 
membrane. Presence of additives improves the 
viscosity of the solution. The pure water permeation 
rate is found to be significantly higher for M 
compared to M-1.Incorporation of additives in the 
casting solution generally increase the water 
permeation rate. It can be observed from the several 
castings that exposure to higher ambient humidity 
gives more porous membranes with higher water 
permeation rate in all the cases it happens due to partial 
phase separation during membrane casting. It can be 
seen that the permeate flux as well as solute separation 
increase in applied pressure range studied.We have 
studied two characteristics (thickness, porosity) of 
casted membranes & remaining characteristics of the 
membrane can be studied in future. 
REFERENCES 
[1] “Encyclopedia of Polymer science and 
Technology” 3rd Edition Vol 
[2] Mark C. Potter; Handbook of industrial 
membrane technology, No Yes publications. 
[3] Mohr; Membrane application and research in 
food processing. 
[4] Richardson Coulson; chemical engineering, 
volume 2, second edition; Tata McGraw hill 
publishers, USA. 
[5] KatarzyanaMajewska- 
1989, Elseveir science publishers, Page no. 83 
95. 
[6] Synthetuc Polymeric Membrane 
,Robert E.Kistinkg and Irvine California, A 
Wiley-Interscience Publication 
[7] Miss. ShilpaChitnis, Miss. Deval Desai, Miss 
VinayaPrabhu; A project report on Kinetic study 
of PAN membrane by phase inversion 
49 
ence M-2 as 
eate Vol-3 Page(184-245) 
Nowak; Desalination, 
– 
,2nd Edition 
ience inversion, 1997 – 98.
International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 
E-ISSN: 2321-9637 
50 
[8] MunirCheryan; Ultrafiltration and Microfiltration 
handbook; 1998; Tchnomic publishing company. 
[9] Wenli Han, Harry P Gregar, Eli M. Pearce; 
Acrylonitrile copolymers, synthesis 
characterization and formation of ultrafiltration 
membranes; capanneli et al (1983); Page no. 1271 
– 1277. 
[10] B. W. Baker, Membrane Technology & 
Applications, John Wiley & Sons, Ltd.

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Paper id 23201432

  • 1. International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 E-ISSN: 2321-9637 39 Preparation, Characterization and Application of Ultra Filtration (UF) Membranes Rajesh Tripathy Department of Chemical Engineering, G H Patel College of Engineering & Technology, BakrolRoad,Vallabh Vidyanagar-388 120.Gujarat. India. Email: rajeshchemtech@gmail.com Abstract-In recent years, membranes and membrane separation techniques have grown from a simple laboratory tool to an industrial process with considerable technical and commercial impact. Today, membranes are used on a large scale to produce potable water from the sea by reverse osmosis, to clean industrial effluents and recover valuable constituents by electro dialysis to fractionate micro molecular solutions in the food and drug industry by ultra filtration, to remove urea and other toxins from blood stream by dialysis in an artificial kidney, to recover valuable products from waste like protein from waste whey and to release drugs such as scopolamine, nitroglycerine etc. at a predetermined rate in medical treatment.Although membrane processes may be very different in their mode of operation in the structures used as separating barriers. In many cases, membrane processes are faster, more efficient and more economical than conventional separation techniques such as distillation, extraction, adsorption, and absorption.[1,8] Index Terms-commercial impact, scopolamine, nitroglycerine, ultrafiltration 1.0 INTRODUCTION Membranes have gained an important place in chemical technology and are used in a broad range of applications. The key property that is exploited is the ability of a membrane to control the permeation rate of a chemical species through the membrane. In controlled drug delivery, the goal is to moderate the permeation rate of a drug from a reservoir to the body. In separation applications, the goal is to allow one component of a mixture to permeate the membrane freely, while hindering permeation of other components. This paper provides a general introduction to membrane science and technology and cover Preparation, Characterization and Application of Ultra Filtration (UF) Membranes, that is topics that are basic to all membrane processes, such as transport mechanisms, membrane preparation, and boundary layer effects, cover the industrial membrane separation processes, which represent the heart of current membrane technology .Carrier facilitated transport is covered next, followed by reviewing the applications of membranes. The paper closes with that describes various minor or yet tobedeveloped membrane processes, including membrane reactors, membrane contactors for the separation of protein from different west, before disposal. 1.1 Membrane Separation Processes All the membrane technologies are essential separation technologies depending upon size of the constitutes to be separated or on the ionic charges or absence of charges, diffusion into the matrix or some such transport phenomena. Keeping this in mind it is essential to mention here that none of the membrane technologies destroy the pollutants; they either separate or concentrate them for further easy handling. Membranes can be classified into 4 categories depending on the size of the materials they remove from the carrier liquid. The 4 categories, listed from the largest to the smallest pore size, are (a)Micro Filtration (MF) (b)Ultra Filtration (UF) (c)Nano Filtration (NF) (d)Reverse Osmosis (RO) a) Microfiltration (MF):MF is a low-pressure membrane process (0.3 to 3.3 bar) that removes particulate material ranging in size from 0.1 to 1.0 microns (1,000 to 10,000 angstroms) and larger. MF is used for separating suspended or colloidal materials from a feed stream. Water, salts, and selected macromolecules pass through the semi-permeable membrane, and suspended solids are progressively concentrated. In the case of water, bacteria (like Escherichia coli, Cryptosporidium parvum, or Giardia lamblia) can be separated from water with this
  • 2. International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 E-ISSN: 2321-9637 40 technique. The salient features of the process are that it involves no phase change and it is relatively a low energy process. b) Ultrafiltration (UF):UF is a low-pressure membrane process (0.5 to 10 bars) that separates materials in the 0.001 to 0.1 micron range (10 to 1,000 angstroms). UF is used for the separation of high molecular weight dissolved materials (solute). Water, salts, and low molecular weight species selectively pass through the semi-permeable membrane, and macromolecules and suspended solids are retained (progressively concentrated). UF separates bacteria and viruses from the water stream that MF passes because the pore size is smaller. c) NanoFiltration (NF):NF is a high-pressure membrane process used for separating materials less than 0.001 microns (10 angstroms) in size. NF is used for the separation of dissolved materials (solute). Less expensive, NF is not as fine a filtration as RO, but it also requires less energy to perform the separation (i.e. less operation & maintenance cost). In water, NF is very effective in removing hardness (multiple-charged ions), total dissolved solids, and natural organic material (Disinfection-By-Product DBP precursor material) with MF pre-filtration. NF is also known, in the water markets, as the "Membrane softening". d) Reverse osmosis (RO):RO membranes have the smallest pore structure, with pore diameter ranging from approximately 5-15 A0 (0.5 nm - 1.5 nm). The extremely small size of RO pores allows only the smallest organic molecules and unchanged solutes to pass through the semi-permeable membrane along with the water. Greater than 95-99% of inorganic salts and charged organics will also be rejected by the membrane due to charge repulsion established at the membrane surface. 2.0 MATERIALS FOR MEMBRANE MANUFACTURING Pressure driven membrane separation processes fall into four broad categories: microfiltration, ultrafiltration, nanofiltration and reverse osmosis. The materials used for the preparation of these membranes, their morphological characteristics as well as their applications are different from each other. Morphologically the membranes are essentially porous in nature. Pore size in case of microfiltration membranes is in the order of 200 A0 (0.02 microns) to 1,00,000 A0 (10 microns); in ultrafiltration the pore size is between of 20A0-200A0; in nanofiltration it is in the range of 10A0-20A0 and in the case of reverse osmosis it is between 1A0-10A0. Mechanisms of separation are also different for these membrane processes. While size based separations occur in case of microfiltration and ultrafiltration, membrane-solute interaction is the basis in nanofiltration and reverse osmosis. Application wise, microfiltration is used for the separation of solutes having molecular weight more than 3,00,000 Daltons, ultrafiltration is used for solutes in the range of 500-3,00,000 Daltons, nanofiltration is used for separation of solutes with a molecular weight range of 300-500 Daltons and reverse osmosis is used for the separation of solutes with molecular weight up to 300Dalton. Microfiltration is used for separation of suspended materials, coarse colloids, etc., ultrafiltration is useful in case of separation of soluble macromolecules, sugars, proteins, etc., nanofiltration is used in the separation of multivalent ions and reverse osmosis is used for the separation of ionic solutions. The membranes are predominantly polymeric in nature and is thin sheet like materials having typical thickness of the order of 100 microns. It forms a physical barrier between the fluids on either side, yet keeping communication between them. The crucial feature of a particular membrane is its selective permeability to certain species for which certain force is needed for the movement of species through the membrane. The overall driving force in the transport of species across the membrane is the chemical potential gradient, which is the sum of existing gradients such as concentration, pressure and electrical potential. In RO, water molecules are forced through the membrane by applying pressure. Material used for membranes are predominantly polymeric in nature. For RO, polymers such as cellulose acetate, polyamide, polyimide deposited on polysulphone base support etc. are used, whereas in ultrafiltration, the membrane used is made up of polysulfone and poly acrylonitrile.[7] 2.1 Membrane Materials: These can be classified as (a) inorganic and (b) polymeric.
  • 3. International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 E-ISSN: 2321-9637 41 (a) Inorganic: Typical are gamma-alumina, alpha-alumina, borosilicate glass, pyrolyzed carbon, Zirconia/s. steel Zirconia/ carbon, etc. Other types of ceramic membranes are also being developed. Inorganic membranes have certain advantages over polymeric ones, like temperature and chemical stability. The cost of these materials and packing density (area /volume ratio) being the main restriction towards their large -scale applications. (b) Polymeric: typical materials, for Ultrafiltration are polysulphones, polyethersulphone cellulosic materials polyvinylidenefluoride, polyacrylonitrile, polyamides, etc the membranes are typically made by the phase inversion method. Behavior, performance, and limitations of some of the polymeric membrane are given below [1,2] 1) Cellulose Acetate (CA) Raw material used is cellulose, which undergoes acetylation in presence of acetic anhydride, acetic acid and sulphuric acid. It is extensively used in UF studies as it is easy to fabricate less costly high salt retention and relatively high flux .The raw material cellulose is a renewable source. But it also has some drawbacks. Firstly it has fairly narrow range and maximum temperature recommended is 30 0C. This creates problems in maintaining sanitary condition and give lower flux .The PH range is also restricted between 2- 8. Under acidic conditions polymer hydrolyses & structural integrity is lost. Under highly alkaline condition, deacetylation occurs, which will affect selectively, permeability. Also cellulose acetate has a poor resistance to chlorine .It also undergoes compaction and creep to a slightly greater extent pressure. Cellulose acetate is also biodegradable and hence storage properties. 2) Aromatic polyamides (PA) It is also an important material for UF .It is characterized by the having an amide bond in its structure (--CONH--). In general they show good temperature resistance even up to 80 0C .The PH resistance is also good between range 3-11 at 25 0C .PA membranes are not biodegradable. Cleaning PA with acid caustic solutions is feasible but they are more sensitive to chlorine to CA and only polybenimidazole appears to show some resistance. 3) Polysulfone (PS) PS is most widely used in UF. These membranes are characterized by having in its structure diphenylenesulfonerepeating units.It has wide temperature limits from 750C –1250C. Wide PH tolerance from 1-13. It has fairly good resistance and also it is not biodegradable. It is easy to fabricate membranes n wide variety of configurations and wide range of pore sizes. Cleaning using acids and bases and disinfections, using chlorine and H2O2 are feasible. PS is also resistant to strong oxidizing agent. Polysulfone has the apparent low-pressure limit. 4) PAN (Polyacrylonitrile) PAN is hydrophilic in nature. It is not affected by boiling water .It is not affected by weak acids, weak alkalis but affected by strong acids & alkalis. It can be used up to 180 0C.Oxidising agent & common organic solvents have little effect. PAN membranes are hard, relatively insoluble & high melting material. 5) Polyethersulfone (PES): PES is an amorphous material with a translucent amber tint. It has excellent dimensional stability and very good electrical insulation properties. It is also characterized by its creep resistance - substantial loads can be carried for long periods at temperatures up to 180°C - and thermal stability PES parts can be used for thousands of hours up to 200°C with no significant loss of strength. It has relatively high water absorption and, in common with many other plastics, drying is essential before e.g. thermoforming. It has poor fatigue characteristics and is prone to environmental stress cracking but has good long-term thermal ageing resistance and reasonable radiation resistance. 2.2 Selection Of Material It is evident that for selecting a membrane material which would be the best choice, it is necessary to consider operating condition like temperature, pressure; the nature of feed stream i.e. the pH, viscosity, density etc. and other factors like solid contents clean ability. Although the inorganic materials are having more temperature and pressure resistant, they can be used in very high or very low pH, we have chosen polymer membrane for casting and to study performance because polymer membranes are flexible in nature and can be casted in any shape but not the inorganic materials. Inorganic membranes are more tough cannot be casted easily.
  • 4. International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 E-ISSN: 2321-9637 42 There are many polymer membrane materials as discussed above but we have chosen polyethersulfone as a casting material because lot of study is done on other materials but polyethersulfone is not yet explored much as compared to other materials. Before going into details of the casting and performance study we will see some important physical and chemical properties of the polyethersulfone. Membrane materials characteristics a. The ideal membrane has the following characteristics: b. High water flux rates c. High salt rejection d. Tolerance to chlorine and other oxidants e. Resistance to biological attacks f. Resistance to Fouling by colloidal and suspended material g. Inexpensive h. Mechanical strength i. Chemical stability 2.3 Membranes Used in present work : Polymeric - polysulfone/poly(ether sulfone)/sulfonatedpolysulfone - poly(vinylidene fluoride) - polyacrilonitrile - cellulosics - polyimide/poly(ether imide) - aliphatic polyamides - polyetheretherketone Ceramic - alumina (Al2O3) - zirconia (ZrO2) Solvent Used: -Dimethylformamide(DMF) -N, N-Dimethylacetamide.(DMAC) -Dimethylsulfoxide (DMSO) -N-Methylpyrrolidone(NMP) -Morfoline 3.0Membrane Preparation Technique Anumber of different techniques are available to prepare synthetic membranes. Some of these techniques can be used to prepare organic (polymeric) as well as inorganic membranes. The most important techniques are: a. Sintering b. Stretching c. Track-etching d. Phase Inversion e. Coating Most commercially available membranes are obtained by phase inversion. This is a very versatile technique allowing all kind of morphologies to be obtained. This preparation technique is detailed as follows. Phase inversion is a process where a polymer is transformed in a controlled manner from a liquid to a solid state. The process of solidification is very often initiated by the transition from one liquid state in to two liquids (liquid0liquid demixing). At a certain stage during demixing one of the liquid phases (high polymer concentration phase) will solidify so that matrix is formed. By controlling the initial stage of phase transition the membrane morphology can be controlled, i.e., porous as well as nonporous membranes can be prepared. It covers different techniques like a. Solvent evaporation b. Precipitation by controlled evaporation c. Thermal precipitation d. Precipitation from the vapour phase e. Immersion precipitation The most commercially available membranes are prepared by immersion precipitation: a polymer solution (polymer + solvent) is cast on a suitable support and immersed in a coagulation bath containing a nonsolvent. Precipitation occurs because of the exchange of the solvent and nonsolvent. The membrane structure ultimately obtained results from the combination of mass transfer and phase separation.
  • 5. International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 E-ISSN: 2321-9637 43 3.1 Phase Inversion Process Of Membrane Manufacture: This refers to a method of manufacturing asymmetric membranes that result in a “solvent cast structure, which owes it porosity to immobilization of the polymer gel prior to complete solvent evaporation or depletion. This is accomplished by not allowing the cast solution to evaporate to dryness before its structure is set; partial solvent loss occurs so that the solution separates into two interspersed liquid phases. One of these phases represents the voids. As evaporation is allowed to continue, gel structure is set”. [1,8] The steps involved in preparation of Polysulfone membrane are, a. Preparation of polymer solution. b. Casting c. Gelation d. Annealing. Preparation of polymer solution The major constituents of Polysulfone membrane are classified into three types a) polymer base b) solvent and c) swelling agents (magnesium perchlorate or formamide). In addition few more chemicals may be added imparts certain properties of the membranes. Sometimes filler chemicals are also added with co-polymers to form better polymer chain links and improve mechanical strength. A clean, dry, glass beaker, washed with hydrochloric acid, is taken. It is then rinsed with acetone and kept to dry. The specific quantity of Polysulfone is poured into the beaker, which is followed by dimethylformamide. The stirring is stated at this point in order to get a homogeneous material. The remaining chemicals are then added slowly under continuous stirring using a glass stirrer. Proper care was taken to prevent the evaporation of solvents during the process. The polymerization was carried out for 4-5 hours. After this period, a viscous solution with lots of air bubbles trapped in it is obtained. The air bubbles trapped in it are removed by keeping the solution still for 3-4 hours. Thus a clear viscous solution is obtained Casting: The casting of Polysulfone membrane is done in a module. E.g. Flat sheet membranes are made by drawing the polymer solution over a glass plate using a “thin layer chromatography unit”. When this solution is cast and the solvent allowed to evaporate, it results in an increased concentration of polymer at the solution/ air interface, since solvent is lost more rapidly from the surface. The polymer essentially goes out of solution at the surface and forms the so-called skin layer that is characteristic of asymmetric membranes. (This phenomenon is analogues to “case hardening” in products that have been rapidly dried.). After the skin forms, the remaining solvent in the bulk of the mixture evaporates more slowly. Eventually the swelling agent in the mixture starts separating out as a different phase, resulting in two phases within the substructure: the polymer solvent as the concentrated phase and the swelling agent as the dispersed phase. Gelation: The polymer film this formed is further consolidated by a process of gelation. Here, the polymer chain is uniformly linked and distributed in the proper orientation for flow of permeate. Gelation is obtained by keeping the membrane in water at a low temperature of about 5-6 oC. Annealing: The polymer film thus produced, having a hard crust layer on spongy porous support, is still mechanically weak and highly compressible. With application of pressure the pores can be easily stretched. These are hardened with consequent shrinkage of pores by means of proper heat treatment of the membrane. This can be achieved by the process of annealing.The peeled sheet is immersed in hot water for a period of five minutes; the membrane is maintained at 70oC. Product flux and solute rejection can be controlled buy a process condition of this step. Higher temperature causes a decrease in flux of product water and an improvement in solute rejection and vise –versa. Since the degree of rejection can be adjusted by changing the heating temperature, this step is very important in membrane preparations. 3.0 RESULTS AND DISCUSSION 3.1 Analysis of Protein Solution To study the performance of ultrafiltration membrane experimentation is done on dairy whey /milk/protein solution .In this report, to study the performance of PS membrane which are casted in laboratory, the standard protein solution is used. The concentration of BSA protein solution used for experimentation is 0.5%.
  • 6. International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 E-ISSN: 2321-9637 44 0.4 0.35 0.3 0.25 0.2 0.15 0.1 0.05 0 0 0.2 0.4 0.6 Absorbance protein conc. (%) Series2 Linear (Series2) First of all protein solution is prepared, then by biuret method calibration chart is plotted. Then this calibration chart is used for determination of concentration of permeate. The standard protein solution is prepared as follows, 1. Preparation of standard BSA solution Take 50 mg of BSA protein powder in conical flask and dilute it in 10 ml of distilled water. Then the standard protein solution i.e. the solution having 0.5 % concentration will be ready for membrane characterization. First of all by using this BSA solution one can plot a calibration curve, which will be helpful for the analysis of permeate obtained stirred cell apparatus. 3.2. Analysis of BSA by Biuret Method a) Preparation of biuret reagent: Dissolve 9 gms. of sodium potassium tartarate in approximately 400 ml of 0.2 N NaOH. Dissolve separately 3 gm of CuSO4.H2O in minimum quantity of distilled water & transfer slowly with constant stirring to sodium potassium tartarate. Then add 5 gm of potassium iodide & adjust the whole solution to 1000 ml by addition of 0.2 N NaOH. b) Preparation of calibration chart: Six test tubes were taken. A sample of BSA solution of 0.5% concentration and water were prepared in six test tubes according to the table given. And four ml of biuret reagent was added in each test tube. Incubate this solution at room temperature for ½ an hour and absorbance was measured at 530 nm for the respective samples in spectrophotometer. The respective absorbance with different concentration of protein solution is shown in table 5.1. Now the absorbance at the respective concentration is known so the calibration curve between absorbance and protein concentration is drawn as shown in figure 1. Table .1 Calibration chart. Std .BS A ml Distille d water ml Biuret Reage nt ml Protein concentrati on (wt/vol) % Absorban ce At 530 nm 0.0 1.0 4 0.0 -- 0.2 0.8 4 0.1 0.094 0.4 0.6 4 0.2 0.2 0.6 0.4 4 0.3 0.217 0.8 0.2 4 0.4 0.283 1.0 0.0 4 0.5 0.333 Figure 1. Calibration Curve From this calibration curve concentration of permeate (less than 0.5% concentration) can be obtained. This calibration curve has a limitation that conc. more than 0.5% can not be taken in a feed as the curve shows straight line nature up to 0.5% concentration. 3.3 Stirred cell Apparatus Construction: The stirred cell apparatus consist of [1] a. Cell cylinder b. Pressure gauge c. Compressor d. Magnetic stirrer A] Cell cylinder: It consists of a. Pressure inlet: For applying pressure to feed. b. Pressure release valve: To release pressure in the cell cylinder. c. Transparent acrylic body. d. O – ring: To fit the membrane on membrane support. e. Stirring bar: For stirring of solution. f. Membrane g. Membrane support: To fit the membrane in cell cylinder. h. Filtrate out: To collect the permeate. B] Pressure gauge: It is used to apply the pressure inside the cell. C] Compressor: Compressed air is sent at 1 – 2 kg/cm2 in cell cylinder. D] Magnetic stirrer: Cell cylinder is mounted on magnetic stirrer which in tern is used to stir the stirring bar placed inside the cell cylinder.
  • 7. International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 E-ISSN: 2321-9637 45 Figure 2. (a) Stirred cell Apparatus schematic diagram Figure 2.(B)Working model of Stirred cell ApparatuswithUltrafiltration of BSA Protein solutions. Working: Part A: Measurement of Distilled water flux. Take 50-60 ml of distilled water in stirred cell. Start magnetic stirrer. Maintain moderate rpm. Start Air compressor and maintain the pressure on the pressure gauge as 1 Kg/Cm2 .As soon as the pressure is developed, start the stopwatch. Note down Time required to collect 1 ml of permeate. Take 30-40 readings. Part B: Measurement of BSA Protein solution flux/ milk flux/Whey Flux. Take 50-60 ml of known concentration of protein solution/whey/milk as feed solution in stirred cell. Start magnetic stirrer. Maintain moderate rpm. Start Air compressor and maintain the pressure on the pressure gauge as 1 Kg/Cm2 .As soon as the pressure is developed, start the stopwatch. Note down Time required to collect 1 ml of permeate. Take 30-40 readings. Part C: Measurement of volume concentration factor. The stirred cell experiment as mentioned in measurement of BSA protein solution flux was performed. After 5 minutes amount of permeate collected was noted and after each 4 ml time required was noted. 3-4 readings were taken. VCF is calculated by,VCF= volume of feed / volume of rententate Part D: Measurement of Rejection The standard stirred cell experiment for BSA protein solution was performed and after 4 ml time required to collect permeate was noted and flux is calculated. The absorbance of each 4ml permeate was noted and overall absorbance was noted. Permeate concentration was calculated from the calibration curve. The Rejection is calculated by R = 1-Cp / Cf Where,Cp: Concentration of permeate in % wt / vol Cf: Concentration of feed in % wt / vol 4.0 MEMBRANE CHARACTERIZATION 1. Thickness: The thickness of standard UF membrane ranges from 20 – 100 micron. The thickness of casted membrane is measured with the help of micrometer screw gauge at different points on the membrane and the average thickness is calculated. It is used in the measurement of pore diameter and porosity. 2. Porosity: Porosity is the ratio of pore volume of the membrane to the total volume of membrane. It is calculated as follows, 1. Take wt. of wet membrane (in water). 2. Dry the membrane in oven for few minutes & take its dry weight. 3. Take the difference & multiply with density of water that will give you the pore volume of membrane. 4. From area & thickness of membrane calculate volume of membrane.
  • 8. International Journal of Research in Advent Technology, Vol.2, No. 5. Ratio of pore volume to membrane volume will give you porosity. Porosity = pore volume/ membrane volume 5 .0 MATERIALS AND METHODS 5.1. Materials Polysulfone (PS) in powder form was obtained from M/s. Gharda Chemicals Company, India. The solvents used for membrane making are N,N formamide (DMF) and were of reagent grade. Polyethylene glycol (PEG), Polyvinyl Pyrrolidone (PVP K-30) of different molecular weights and piperazine (AR grade) were locally procured and used as additives. 5.2. Preparation of membrane In airtight glass bottle, a specified quantity of polymer was taken and then a known quantity of the solvent was added. The solution w for several hours for complete dissolution.Calculated quantities of additives were subsequently added and the solution was homogenizedand kept for deairation. The solution viscosity was measured using a standard Brookfield viscometer.The dope solution thus obtained was spread over a smooth glass plate with the help of a knife edge. The thickness of the membranes was controlled by varying the thickness of adhesive tapes at the sides of the glass plate. The glass plate was kept in an environment of controlled temperature and humidity during membrane casting. No deliberate solvent vaporation period was allowed. The glass plate was subsequently immersed in a gelling bath, which is generally demineralized water maintained at a known temperature otherwise as mentioned in the text.Immediately phase inversion starts and after fewminutes thin polymeric film separated out from the glass. It was repeatedly washed with demineralized water and wet stored. The actual thickness of the membranes was measured using a micrometer. Table 2. Dope solution compositions Dop e PS Compositio n in Wt. % PS Solutio n DMF Additiv M 1 16 84.9 M 2 16 80.6 M 3 16 74.3 E-ISSN: 2321-9637 N-dimethyl nt was kept agitated ope ent therwise e 1 Wt. % Additiv e 2 Wt. % 0 3.5 4 3.5 10 3.5 Sl No Volume DW 1 ml M 1.1 BSA 1 0-5 BSA 2 05--10 BSA 3 10--15 BSA 4 15-20 M 1.2 P Whey1 0-5 P Whey2 05--10 P Whey3 10--15 P Whey4 15-20 Results of M-1 in ml Time in Sec Table 3.Effect of the time on the Membrane Flux Figure 3.Effect of the time on the performance of Membrane Flux Figure 4.Effect of the time on the performance of Membrane Flux 3, March 2014 46 performance of model M 1.1 model M 1.2 Flux lt/hr.m2 190 20.105 212 18.019 267 14.307 295 12.94 308 12.4 493 7.74 520 7.34 551 6.93 606 6.303
  • 9. International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 E-ISSN: 2321-9637 47 Table 4. Effect of the Pressure on the performance of Membrane Flux Sl No Pressure kg/cm2 Time in Sec Flux lt/hr.m2 M1.3 DW 1 0.50 306 12.48 DW 2 1.00 190 20.1 DW 3 1.20 180 21.22 DW 4 1.40 163 23.43 M1.4 BSA 1 0.50 277 13.79 BSA 2 1.00 213 17.93 BSA 3 1.20 185 20.64 BSA 4 1.40 160 23.87 25 20 15 10 5 Figure 5.Effect of the Pressure on the performance of Membrane Flux M 1.3 30 25 20 15 10 5 Figure 6.Effect of the Pressure on the performance of Membrane Flux M 1.4 Results of M-2 Table 5.Effect of the time on the performance of Membrane Flux Sl No Volume in ml Time in Sec Flux lt/hr.m2 DW 1 ml 19 201.05 M 2.1 BSA 1 0-5 52 73.46 BSA 2 05--10 70 54.57 BSA 3 10--15 90 42.44 BSA 4 15-20 103 37.08 M 2.2 P Whey1 0-5 109 35.046 P Whey2 05--10 151 25.29 P Whey3 10--15 163 23.43 P Whey4 15-20 174 21.95 80 70 60 50 40 30 20 10 Figure 7..Effect of the time on the performance of Membrane Flux M 2.1 40 35 30 25 20 15 10 5 Figure 8.Effect of the time on the performance of Membrane Flux M 2.2 M 1.3 0 0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 Pressure in Kg/cm2 F lu x M 1.4 0 0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 Pressure in Kg/cm2 F lu x M 2.2 0 0 20 40 60 80 100 120 140 160 180 200 Time in Sec F lu x M 2.1 0 0 20 40 60 80 100 120 Time in Sec Flux
  • 10. International Journal of Research in Advent Technology, Vol.2, No. Table 6.Effect of the Pressure on the performance of Membrane Flux Figure 9. Effect of the Pressure on the performance of Membrane Flux M 2.3 Figure 10.Effect of the Pressure on the performance of Membrane Flux M 2.4 Sl No Pressure kg/cm2 Time in Sec M 2.3 DW 1 0.50 33 DW 2 1.00 19 DW 3 1.20 16 DW 4 1.40 12 M 2.4 BSA 1 0.50 148 BSA 2 1.00 58 BSA 3 1.20 52 BSA 4 1.40 50 E-ISSN: 2321-9637 Results of M-3 Table 7. Effect of the time on the performance of Membrane Flux Sl No Volume in ml DW 1 ml M 3.1 BSA 1 0-5 BSA 2 05--10 BSA 3 10--15 BSA 4 15-20 M 3.2 P Whey1 0-5 P Whey2 05--10 P Whey3 10--15 P Whey4 15-20 Figure 11. Effect of the time on the performance of Membrane Flux M 3.1 Figure 12. Effect of the time on the performance of Membrane Flux M 3.2 Flux lt/hr.m2 115.75 201.05 238.75 318.33 25.81 65.85 73.462 76.4 3, March 2014 48 Time in Sec Flux lt/hr.m2 26 146.92 90 42.44 144 26.52 160 23.87 179 21.34 192 19.89 230 16.6 283 13.49 310 12.32 .
  • 11. International Journal of Research in Advent Technology, Vol.2, No. Results of M-3 Table 8.Effect of the Pressure on the performance of Membrane Flux Sl No Pressure kg/cm2 Time in Sec M 3.3 DW 1 0.50 38 DW 2 1.00 26 DW 3 1.20 20 DW 4 1.40 18 M 3.4 BSA 1 0.50 87 BSA 2 1.00 75 BSA 3 1.20 64 BSA 4 1.40 60 Figure 13.Effect of the Pressure on the Membrane Flux M 3.3 E-ISSN: 2321-9637 Flux lt/hr.m2 100.52 146.92 191 212.22 43.9 50.93 59.93 63.66 performance of 3, March 2014 Figure 14.Effect of the Pressure on the performance of Membrane Flux M 3.4 6.0 CONCLUSION AND FUTURE SCOPE Aseries ofUtrafiltration PS membrane was successfully casted & performance was studied for M– M 1,M– 2 and M – 3 (distinction based on polymer concentration and additive concentration and the effect with different solvents).Stirred cell operation was performed with standard Bovoin Serum Albumin (BSA) protein solution (0.1 % concentration).,Distilled water flux, Dairy Waste with different pressure range starting from 0.5-1.4 kg /cm2.We have observed that for three membranes as the time increases flux goes on decreases due to fouling.Rejection increases with increase in PS concentration in ultrafiltration membrane. Presence of additives improves the viscosity of the solution. The pure water permeation rate is found to be significantly higher for M compared to M-1.Incorporation of additives in the casting solution generally increase the water permeation rate. It can be observed from the several castings that exposure to higher ambient humidity gives more porous membranes with higher water permeation rate in all the cases it happens due to partial phase separation during membrane casting. It can be seen that the permeate flux as well as solute separation increase in applied pressure range studied.We have studied two characteristics (thickness, porosity) of casted membranes & remaining characteristics of the membrane can be studied in future. REFERENCES [1] “Encyclopedia of Polymer science and Technology” 3rd Edition Vol [2] Mark C. Potter; Handbook of industrial membrane technology, No Yes publications. [3] Mohr; Membrane application and research in food processing. [4] Richardson Coulson; chemical engineering, volume 2, second edition; Tata McGraw hill publishers, USA. [5] KatarzyanaMajewska- 1989, Elseveir science publishers, Page no. 83 95. [6] Synthetuc Polymeric Membrane ,Robert E.Kistinkg and Irvine California, A Wiley-Interscience Publication [7] Miss. ShilpaChitnis, Miss. Deval Desai, Miss VinayaPrabhu; A project report on Kinetic study of PAN membrane by phase inversion 49 ence M-2 as eate Vol-3 Page(184-245) Nowak; Desalination, – ,2nd Edition ience inversion, 1997 – 98.
  • 12. International Journal of Research in Advent Technology, Vol.2, No.3, March 2014 E-ISSN: 2321-9637 50 [8] MunirCheryan; Ultrafiltration and Microfiltration handbook; 1998; Tchnomic publishing company. [9] Wenli Han, Harry P Gregar, Eli M. Pearce; Acrylonitrile copolymers, synthesis characterization and formation of ultrafiltration membranes; capanneli et al (1983); Page no. 1271 – 1277. [10] B. W. Baker, Membrane Technology & Applications, John Wiley & Sons, Ltd.