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International Journal of Engineering & Technology IJET-IJENS Vol:13 No:02

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A Review: Development of Polymeric Blend


Membrane for Removal of CO2 from Natural Gas
Asim Mushtaq*, Hilmi Bin Mukhtar, Azmi Mohd Shariff, Hafiz Abdul Mannan
Department of Chemical Engineering
Universiti Teknologi PETRONAS
MALAYSIA
engrasimmushtaq@yahoo.com, hilmi_mukhtar@petronas.com.my,
azmish@petronas.com.my,mannan1403@hotmail.com

Abstract

In this paper, natural gas also referred to as,


Princess of Hydrocarbon. As it is a fastest growing energy
source, gas separation membranes are extensively used for the
separation of CO2 from natural gas. Polymeric membranes have
mechanical strength, reproducibility and economical processing
capacity. However they suffer from upper bound tradeoff
between permeability and selectivity. Inorganic membranes have
high selectivity, robustness, thermal and chemical stability but
these membranes are economically unfavorable due to high
capital and maintance cost. In mixed matrix membrane (MMM)
superior gas separation properties of inorganic membranes and
economical processes ability of polymeric membranes are
exploited by combining the inorganic particles in polymer
matrix. In case of glassy polymer, poor distributions of dispersed
phase in polymer matrix and week contact of particles in
polymer matrix are the challenges in MMM. For rubbery
polymers, poor selectivity of MMM is the core problem. Blending
of a glassy and a rubbery polymer with amines is suggested to
develop a polymeric blend membrane by coating the polymer
blend with different amines of high selectivity and permeability.
The developed membrane will be characterized and its
performance will be evaluated for the separation of CO2 from
natural gas in terms of selectivity and permeability.

Index Term-- Natural Gas Purification, Carbon Dioxide


Removal, Polymeric Blend Membrane, Selectivity, Permeability.

I.
INTRODUCTION
Natural gas, called the Princess of Hydrocarbon and it is
the fastest growing energy source in the world. It is used as a
main fuel such as residential like for cooking the food,
industrial like as raw material for Petrochemicals and
Fertilizer industries, transportation like CNG and it also used
in many commercial areas like generating electricity. The
presence of CO2 in natural gas lower down its calorific value
for incomplete combustion as well as environmental issues
occur like its emission to atmosphere is increasing Green
House Effects and Global Warming so therefore need to be
removed and increases the worth value. The price of natural
gas varies greatly depending on location and type of
consumer.

Fig. 1. Natural Gas Use By Sector 2011


Source: EIA - Energy Outlook 2012

The composition of natural gas can vary from well to


well due to its geographical condition, but below in a chart
outlining the typical makeup of natural gas before it is refined.
T ABLE I
C OMPOSITION OF N ATURAL GAS [1]

COMPONENT
Methane
Ethane
Propane
Butane
Carbon Dioxide
Oxygen
Nitrogen
Hydrogen
sulphide
Rare gases

FORMULA
CH4
C2H6
C3H8
C4H10
CO2
O2
N2

COMPOSITION
70-90%
0-20%
0-45%
0-0.2%
0-5%

H2S

0-5%

A, He, Ne, Xe

trace

As we discuss previous, CO2 is an acid gas causing


corrosion to the equipment. Also CO2 is a major contributor to
global warming. Moreover it reduces the heating value of

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natural gas and imposes unnecessary transportation cost.
Therefore natural gas must be treated to remove CO 2 to
improve the quality of the product before delivery to the
pipeline [2,3].
In gas separation, the trade off limitations of
polymeric membranes and economical consideration of
inorganic membranes motivated the researchers to search for
alternative approaches. Membranes with high selectivity and
high permeability are required. Different modifications are in
practice to improve the performance of membranes like mixed
matrix, cross linking, grafting, polymer blending, making
composite or hybrid membrane.
But the performance of mixed matrix membrane still
suffers from defects caused by poor glassy polymer- particle
interaction. High critical temperature gases, such as carbon
dioxide, are known to strongly interact with glassy polymers
and have high solubilities in most polymers. Plasticization is,
therefore, especially problematic in natural gas purification.
Rubbery polymers suffer from lack of selectivity and
their performance is below the upper bound limit even at high
inorganic filler loadings. Polymeric materials suffer from
general tradeoff between selectivity and permeability.
In this context polymeric blending with amines offers time
and cost effective method to develop materials with desirable
properties. Therefore effect of blending of a glassy and a
rubbery polymer, then mix the amine with topping of amines
on the performance of polymeric membrane should be
research so that a membrane with high selectivity and high
permeability could be developed.

i.

ii.

II.
ISSUES
In the drilling step, the production of natural gas contains
high impurity contents but it depends on wells to wells.
The most common impurities which are present like
moisture, carbon dioxide, nitrogen, hydrogen sulphide and
traces of metals. These impurities create a environmental
problem as well as combustion problem. The
environmental effects of carbon dioxide are of significant
interest, for example, global warming, ocean acidification
and anthropogenic climate change.

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In this context to develop a Polymeric Blend (glassy/


rubbery/amines) membrane type to increase the
permeability and selectivity.
IV. RESEARCH OBJECTIVES
In order to address the above mentioned problem, the
following objectives will be carried out:

To identify the blending behavior of glassy and rubbery


polymers with amines.
To characterize the developed membrane in order to find
its physico-chemical and thermal properties.
To evaluate the performance of the developed membrane
in terms of selectivity and permeability for the separation
of CO2/CH4 gas mixture.
To develop a new model for prediction of the permeability
of gases and validate the data.
V.
LITERATURE REVIEW
The phenomenon of osmosis was discovered in 1748 and
during the following century, osmosis was of special interest
to practitioners in the biological and medical sciences.
Experimental work was conducted primarily with membranes
of animal (bladder) and plant origin (onion). In 1907 Bechold
introduced term ultrafiltration forcing solutions at pressures
up to several atmospheres through membranes prepared by
impregnating filter paper with acetic acid collodion. By 1950,
Hassler introduced the first concept of membrane desalination
and Loeb-Sourirajan invented so called asymmetric
membrane, which made commencement of practical
membrane applications in 1962.
A. Initial Concept of Membrane Separation
Membrane can be defined as: It is a semipermeable active or
passive barrier which, under a certain driving force, permits
preferential passage of one or more selected species or
components (molecules, particles or polymers) in a gaseous
and/or liquid mixture solution [7,8].
MEMBRANE

CO2 is highly corrosive, especially when react with water


then it corrodes the pipeline and equipment frequently. In
LNG plant, CO2 destroys the pipeline and the
transportation system. It can also reduce the calorific value
and eventually lower the selling price of the gas[4].
Therefore the removal or purification of natural gas is very
important step.

III. PROBLEM STATEMENT


Existing technologies have limitations like high energy
consumption and large area required.
To develop membrane technology for offshore / remote
areas application for natural gas containing high CO2.

FEED

Driving
PERMEATE
Forces: C, p etc.

Fig. 2. Schematic diagram of gas separation process by a membrane

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T ABLE III
INDUSTRIAL APPLICATIONS OF GAS SEPARATION MEMBRANES [5,6]

The primary species rebound back by the membrane is called


retentate or solute, while those species passing through the
membrane is called permeate or solvent which shown in
Figure 2.
There are three different important mechanisms by which
membrane can perform separations:
By having pores which are of such a size that certain
species can pass through and others cannot, this
mechanism is called size exclusion.
By selective retardation by the pores when its diameters
are close to molecular sizes, this mechanism is called pore
flow.
By dissolution into the membrane, movement by
molecular diffusion across the membrane, and reemergence from the other side, called solution diffusion.
The driving force also exists in the form of pressure,
concentration, or voltage difference across the membrane. The
driving force depending on the physical sizes of the separated
species.

GAS SEPARATION
O2/N2

B. Materials for Gas Separation Membrane


The selection of material membrane is the most important
factor for Gas Separation. Chemical interaction between a
membrane material and a gas penetrant determined the
separation efficiency of a membrane separation process [9].
The choice of material is based on the application
and cost-effectiveness. The most important requirements of
effective separation material are:[10,11]
1. Engineering feasibility.
2. Good chemical resistance.
3. High separation efficiency with reasonable high flux.
4. Good mechanical stability.
5. High thermal stability.
6. Low cost.
C.

Industrial Applications of Membrane in Gas Separation


Membrane separation processes have very important role
in separation industry because membrane separation processes
is that it operate without heating. Nevertheless, they were not
considered technically important until mid-1970. The
industrial gas separation is widely spread by using the
membrane in last 25 years. The multiple application of gas
separation membrane is listed in Table III.

APPLICATION
Oxygen enrichment, nitrogen
(Inert gas) generation

Hydrocarbons/H2

Refinery hydrogen recovery

H2/N2

Ammonia purge gas

H2S/Hydrocarbons

Sour gas treating

He/Hydrocarbons

Helium separations

He/N2

Helium recovery

Hydrocarbons from

Organic solvent and monomer

process streams

recovery

H2/CO

Syngas ratio adjustment

Hydrocarbons/Air

The membrane processes are classified as:


Microfiltration (MF) Membrane
Ultrafiltration (UF) Membrane
Nanofiltration (NF) Membrane
Reverse Osmosis (RO) Membrane
The size of materials retained for each process, the driving
force behind separation and the type of membrane.

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Pollution control,
hydrocarbon recovery

H2O/Air

Air dehydration

H2O/Hydrocarbons

Natural gas dehydration

D. Issues and Challenges in Membrane Applications for Gas


Separation
The following issues and challenges occur in membranes
application for gas separation:
Membrane Fouling
High Cost
Concentration of Polarization
Lack of selectivity
Lack of mechanical resistance
Sensitivity to chemical attack
Membrane cleaning
Module Design
E. Membrane Separation Mechanism
In gas separation processes there are two streams ;
Upstreams and Downstreames. Pressure gradient between in
these two streams which occur the separation processes.
Permeation is a rate-controlled process and separation degree
is determined by the selectivity of membrane at the conditions
of separation, including temperature, pressure, flow rate, and
area of membrane[12]. The membrane separate gases only,
some component passes more rapidly than the other, it also
depends upon the pore size.
There are four fundamental transport membrane separation
mechanisms are:
1.
2.
3.
4.

Poiseuille flow
Knudsen diffusion
Molecular sieving
Solution-diffusion.

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temperature. The molecules can start to wiggle around at


this temperature. The polymer now is in its rubbery state.
The rubbery state tends to softness and flexibility to a
polymer.

Fig. 3. Schematic presentation of main mechanisms of membrane-based gas


separation [13]

F. Polymeric Membranes
Polymeric membranes perform their process by different
mechanisms which are based upon the properties of membrane
means physical and chemical structure. It interaction between
membrane, components and nature of gas[14].
It can be classified into two types: porous and non porous
[15].
A porous membrane is a rigid, highly voided structure
with randomly distributed interconnected pores like a
conventional filter. Separation is dependent on molecular size
of polymer and pore size distribution. These membranes
exhibit high fluxes but they are inherently low selective.
Non porous membrane also called as dense membrane
consists of a dense film. Permeate molecules are first absorbed
and then diffused through polymer matrix under the driving
force of pressure or concentration gradient. Dense membranes
are highly selective but transport of gas through the polymer
medium is very low. Permeate of similar sizes can be
separated by dense membranes if they have significantly
different solubility in polymer.
Polymeric membranes can be classified on the basis on
polymer material.
Glassy Polymer. {At low temperatures molecular motion
in an amorphous region is restricted to molecular
vibrations, but the chains cannot move or rotate in space .
This form is the glassy state of the amorphous region. The
glassy state can be considered as a super cooled liquid
where the molecular motions have been frozen in. The
glassy state is brittle, hard and rigid like a crystalline solid,
but it retains the molecular disorder of a liquid.}[20]. At a
low temperature the amorphous regions of a polymer in the
glassy state, the molecules are frozen on place. They may
be able to fluctuate slightly, but they do not have any
segmental motion in which portions of the molecule
wiggles around. Whenever the amorphous regions of a
polymer are in the glassy state, it generally will be brittle,
hard and rigid.
Rubbery Polymer. {When the material is heated the
polymer will reach a temperature at which segments of the
entangled chains can move. The amorphous region
becomes rubbery at this temperature, which is called the
glass transition temperature. When an amorphous polymer
in rubbery state, it is soft and flexible}[20]. If the polymer
is heated it eventually will reach its glass transition

Semi-crystalline solids have both crystalline and


amorphous regions. Accordingly the temperature, in the
amorphous regions can be either in the rubbery or glassy state.
Temperature at which the transition in the amorphous regions
between the glassy and rubbery state occurs is called the glass
transition temperature.
The amorphous portion of semi-crystalline solid contains
the glass transition property. During the glass transition the
crystalline portion remains crystalline.
There is a general tradeoff between permeability and
selectivity for polymeric membranes with rubbery polymeric
membranes with high permeability and low selectivity and
vice versa for glassy polymeric membranes. Despite their
mechanical strength, reproducibility and economical
processing capacity, dense membranes are still not much
attractive because they suffer from upper bound tradeoff
between permeability and selectivity. Robeson in 1991
proposed this upper bound trade off and is shown in below
figure graph between Permeability and Selectivity.

Fig. 4. Robeson upper bound trade off

This plot shows the selectivity for CO2/CH4 obtained


from the ratio of pure-gas permeabilities plotted against
carbon dioxide permeability for all the membrane materials
then reported. The line that links the most-selective polymers
at a particular carbon dioxide permeability is called the upper
bound, beyond which no material is currently known. The
performance of todays commercial membranes, when used
with high-pressure natural gas, is also shown on this Robeson
plot. Generally, commercial membranes that are in use have
half the selectivity of the best upper bound materials.
Moreover use of polymeric membranes is limited to
separation processes where hot reactive gases are not
encountered because these membranes cant withstand
chemical and thermal attacks [16]. Usually glassy polymeric

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membranes are preferred for CO2 removal because glassy
polymers separate gas mixture on the basis of difference in
molecular size of penetrating molecules and CO2 has a low
molecular size as compared to methane.
G. Comparison of Polymeric, Inorganic and Mixed Matrix
Membranes
A comparison of polymeric, organic and mixed matrix
membrane is given in table in terms of cost, chemical and
thermal stability, and mechanical strength, compatibility to
solvent, swelling, separation performance and handling. It is
clear from the table that polymeric membranes are economical
to fabricate and have good mechanical strength. Their
separation performance and stability is moderate and these are
robust in handling. Their main disadvantage lies in swelling
and compatibility to solvent. However still for industrial
applications polymeric membranes are preferred.
TABLE IV
COMPARISON OF VARIOUS MEMBRANES [17]

Properties

Cost

Polymeric

Inorganic

Mixed matrix

membranes

membranes

membranes

Economical
to fabricate

High
fabrication

Moderate

Moderate

High

High

Good

Poor

Excellent

Limited

Wide range

Limited

Frequently

Free of

Free of

occurs

swelling

swelling

stability
Mechanical
strength
Compatibility
to solvent
Swelling

Exceed
Separation
performance

Moderate

Moderate

Robeson
upper
boundary

Handling

Robust

Different techniques are being used to improve the


performance of polymeric membranes to withstand required
duties. Blending is a cost and time effective method to
develop materials with desired properties. However, blending
of glassy and rubbery polymers has not been studied.
VI. METHODOLOGY
In this study, the main objective is to fabricating a Blending
Membrane which is the combination of polymeric membrane
(Glassy and Rubbery Polymer) and amine solution layer for
natural gas purification. For the fabrication of polymeric
blending membrane we have to follow the two steps:
First we will prepare the polymer blend of polymeric
membrane by the combination of glassy and/or
rubbery polymer.
In the second step a polymer blend mix with amines
to develop the enhanced polymer blend membrane.
In the third step a coating is provider of with different
amines solutions, for that purpose to improve the
separation ability for CO2/CH4 mixture.
In order to find out compatibility of selected polymers, initial
experimentation will be carried out to study blending behavior
of polymers in different solvents. The best compatible
polymer pair will be selected for membrane development.

cost

Chemical &
Thermal

57

Brittle

A. Membrane Casting
Fabrication of membrane will be carried out in two steps by
conventional casting and solvent evaporation method i.e.
Preparation of dope solution and Casting process to form
membrane thin film. Polymers will be dissolved in a solvent at
room temperature under continuous stirring to obtain a
homogeneous mixture. Then this mixture will be casted to
form dense sheets of membranes. Finally annealing will be
applied at elevated temperature to obtain the desired
membrane.
B. Membrane preparation by dry/wet induced phase
inversion process
Polymer blend membranes were fabricated by the dry/wet
phase inversion process. Polymers were pretreated in a
vacuum oven at 100C for 12 h prior to the polymer solution
preparation. The polymer blend compositions of
Glassy/Rubbery were varied from different composition in
solubility
as
solvent.
Membrane
with

Robust

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TABLE V
DIFFERENT STUDIES REGARDING ON BLEND MEMBRANE

S
No

Year

2002

2006

Polymers
PES/PI (Glassy/Glassy)
coated with PDMS
PU based PEI/PAI
(Glassy/Glassy) blend

System

Remarks

Gas separation

Hollow fiber

CO2

PU/PDMS
3

2006

(Rubbery/Rubbery) cross-

gas mixture

linked
studied effect of polymer concentration,

2006

PVDF/PES (Glassy/Glassy)

2009

2008

2010

2010

2010

10

2010

PES/PI (Glassy/Glassy)

O2/N2

11

2011

SPEEK/ Matrimid

CO2 separation

Cross-linked for anti-plasticization

12

2011

PSF/PI (Glassy/Glassy)

CO2/CH4

studied effect of solvents

13

2011

PEI/PVP

CO2/CH4, CO2/N2

Carbon hollow fibre membrane

14

2012

toulene/water

pervaporization

15

2012

PU/PVAc with PEO/PPO

gas mixture

increased CO2 permeability

16

2012

PIM-1/ Matrimid

CO2/CH4 , CO2/N2

increased selectivity

solvent & morphology

PVAm/PVA with porous

faclitated CO2

Ultra-thin membrane with good strength,

PES support

transport

stability and permeability/selectivity

PES/PI (Glassy/Glassy)
blend MMM
PU/PDMS
(Rubbery/Rubbery)
PEG/PDMS
PU/CA(porous)
(Glassy/Rubbery)

PES (PVP or PEG) with


PDMS coating

O2/N2
methanol/toulene

pervaporization

CO2 separation
micro filtration

CA=cellulose acetate, PAI=polyamide imide, PDMS=polydimethyl siloxane, PEA=aromatic polyether amide,


PEG=polyethylene glycol, PEI=polyether imide, PEO=polyethylene oxide, PES=polyether sulfone,
PU=polyurethane, PI=polyimide, PIM-1=polymer of intrinsic microporosity, PPO=polypropylene oxide,
PSF=polysulfone, PVAc=polyvinyl acetate, PVAm=polyavinylamine, PVDF=polyvinylidene fluoride,
PVA=polyvinyl alcohol, PVP=polyvinyl, SPEEK=sulfonated aromatic poly(ether-ether-ketone)

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different polymer concentrations i.e 100%, 75%, 50%, 25%
will be fabricated for comparative study.
Spin casting was done on a glass plate at 850 rpm. Casted
films were evaporated for 30 s under the relative humidity
555% and at a temperature of 24C. Then they were
immersed into the water coagulation bath at 151 C. The
casted membranes were kept in a vacuum oven at 80 C for 1
day to remove the residual solvent present.
C. Polymeric membrane coating with Amine solution
After the fabrication of Polymeric membrane we will add
a topping of Amines. Because the goal of this study to remove
the carbon dioxide from the natural gas. To achieve this goal
we combine the two major separation processes membrane &
Absorption. Membrane has a good ability of separation and
amine has a good ability to absorb carbon dioxide. By the
combination of these two processes we can enhance the
permeability and selectivity.
In this study, when the mixture of gases CO2 / CH4 will
pass through the Polymeric membrane the amine layer absorb
the maximum carbon dioxide and CO2 permeation rate will be
higher in the membrane, and maximum amount of CH4 will
not be absorb in the membrane so the permeation rate of CH 4
in the membrane will be less. So by the following formula the
selectivity of membrane will be increase.

D. Characterization of the Membrane.


The resultant membranes will be characterized in terms of
morphology and physical properties. Characterization of the
developed membrane will be done by different analytical
equipments.
Membrane morphology will be studied by scanning
electron microscope (SEM) and field emission
scanning electron microscope (FESEM).
Thermal and dynamic mechanical properties will be
characterized by dynamic mechanical analysis
(DMA).
To find the amount of residual solvent thermal
gravimetric analysis (TGA) will be used.
Glass transition temperature of membranes and
polymer blend will be measured by differential
scanning calorimeter (DSC)

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Selection of
glassy &
rubbery
materials ,
Solvent &
amines for
membranes

Rubbery
Polymer +
Glassy
Polymer +
Solvent

Polymer Blend
+ Amines

Characterizatio
n of Membrane

Membrane
preparation by
casting
method &
Solvent
Evaporation

Dope Solution

Gas
permeability
Study

Model
development

Model
Validation

Fig. 5. Research Methodology

VII. DISCUSSION
From figure 6, polymer blending offers time and cost effective
method to develop materials with desirable properties.
Therefore effect of blending of a glassy and a rubbery polymer
with different amines solutions, for that purpose to improve
the separation ability for CO2/CH4 mixture. The amine
solution has the capability to purify the natural gas having acid
gas. Amine has a natural affinity for both CO2 and H2S
allowing this to be a very efficient and effective removal
process and also with topping of amines on the performance of
polymeric membrane should be research so that a membrane
with high selectivity and high permeability could be
developed.

BLEND
RUBBERY,
GLASSY&
AMINES

E. Gas Permeability Study


The performance of developed membranes will be studied in a
gas permeation unit in terms of selectivity and permeability
with pure and mixed gas compositions of CO2 at different
pressures.
F. Modeling and Model validation
In this study the modeling will involve for the verification of
experimental results. Different modeling techniques will use
for this purpose.

Fig. 6. Current Trend Of Polymeric Blend Membrane

VIII.
CONCLUSION
The present research addresses the current needs of having
high permeability and selectivity membrane for removal of
CO2 from natural gas. The developed polymer blend

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membranes have improved flexibility, reduced cost, improved
process ability, and enhanced selectivity and/or permeability
compared to the comparable polymer membranes that
comprise a single polymer. It will be possible to develop
polymeric blend membrane for separating high pressure gas
streams at their processing pressure. This advantage could
offer cost savings that may provide a new incentive for
polymeric blend membranes. This result opens a new tool for
studying gas separation by polymeric blend membranes. The
impact of this breakthrough will be able to monetize the
stranded gas wells having high CO2 content. In the future
work we also add the inorganic fillers like carbon molecular
sieves, zeolites in blend, which further enhances the polymeric
blend membrane. Therefore, this will increase the economic
growth in gas industry of the country.

[16] P. Goh, et al., "Recent advances of inorganic fillers in mixed matrix


membrane for gas separation," Separation and Purification Technology,
2011.
[17] A. F. Ismail, et al., "Transport and separation properties of carbon
nanotube-mixed matrix membrane," Separation and Purification
Technology, vol. 70, pp. 12-26, 2009.
[18] M. A. Semsarzadeh and B. Ghalei, "Characterization and gas
permeability of polyurethane and polyvinyl acetate blend membranes
with polyethylene oxidepolypropylene oxide block copolymer,"
Journal of membrane science, 2012.
[19] W. Yong, et al., "Molecular engineering of PIM-1/Matrimid blend
membranes for gas separation," Journal of membrane science, 2012.
[20] Faculty.uscupstate.edu/llever/Polymer%20Resour ces /GlassTrans.htm,
31 Jan 2001

IX.
ACKNOWLEDGEMENT
I would like to express my deep and sincere gratitude to my
supervisor Associate Professor Doctor Hilmi Bin Mukhtar,
for his continued instructive guidance, invaluable suggestions
and unlimited encouragement and support during my review
paper. I am very thank full to NED University of Engineering
& Technology, Karachi Pakistan, who gives the financial
support to me for my higher studies.
[1]
[2]
[3]
[4]
[5]
[6]
[7]
[8]
[9]
[10]
[11]
[12]
[13]

[14]

[15]

60

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