International Journal of Engineering and Technical Research (IJETR)

ISSN: 2321-0869, Volume-2, Issue-5, May 2014

Synthesis of nano structured polyaniline with ionic

and nonionic polymers based enzymatic application
of glucose biosensing
Shatrudhan Palsaniya, Veerender Sharma

used as analyte product i.e. detected. In human body system

Abstract Polyaniline (PANI) a conducting polymer solid enzymes are work as a catalyst which dissociates to the
material stable at room temperature. The nature of aniline glucose in glycogen. This provides internal energy to the
monomer in yellowish colour remains in gel form. The cells and tissue and whole immune system. The chemical
monomer aniline particle remains separate at this gel form. reaction of catalyst enzyme work as a biological recognition
Now aniline polymerized in presence of sodiumdodecylsulfate
element and biological components works as an antigen [3].
(SDS) an ionic surfactant. It entrapped to the aniline monomer
so that the size of nanoparticles got stable manner .A micelles
Mainly electrocatalytic glucose biosensor is depending on the
formation takes place and get swellings, to prevent this glucose oxidase (GOx) enzyme, which catalyzes glucose in
formation we have to mixed ammoniumpersulfate (APS) .It gluconolactone in form of oxidation [4].
does oxidized to the polymerized aniline with Advanced materials are part of the organic compounds [5].
sodiumdodecylsulfate solution. The formation of nano particles Organic compound used with the polymers as conducting
are in spherical in morphological manner at very low monomer polymer materials. Basically polymers are insulator, at this
concentration. Non-ionic polymer Pluronic F-123 is level we have to create a mechanism that they starts conduct,
compositionally synthesized. Now prepared materials are called doping, such type of materials are called conducting
characterized using UV visible spectroscopy, Fourier
polymers and behaves as a semiconductor materials [6-7]. In
transform infrared spectroscopy, XR-D, Scanning electron
microscopy, Atomic force microscopy.. These experiments are
advanced recently such materials has been invented that can
provides strong base to identify the characteristics of be undertake according to the application, means these
nanomaterials ,so that transferring of electrons have fast and materials are case sensitive ,called smart materials.
provide convenience to measure quickly glucose with glucose Conducting polymers have a specific band gap due to that
biosensor. reason they have a property of conduction of electron [8]. In
case of conducting polymers there are three types of
Index Terms concentration activity, Amperometry, Cyclic mechanisms are found i.e. polaron, bipolaron, and solitons
voltammetry, Ag/AgCl and Pt. electrodes, H2O2 electro [8-9]. These are the structures which are responsible for
chemical activity, Glucose Oxidase (Enzyme).
conduction.
I. INTRODUCTION
Conducting polymers used in analytical application like
Sensor is a device which responds to the physical parameters biological parameters. CPs (conducting polymers) works as
in form of sensitivity. Biosensor combines the sensitivity of electrochemical transducer that, converts biological contents
electro analytical methods of the biological components [1]. in to electrical signals. Conducting polymer (PANI) is most
These component senses its catalytic activity which produces prominent materials which is used in biological application
the electrical signals i.e. recognizes by electrodes like, such as biosensors [10]. Because it has greater stability and
transducer which is proportional to the analytic less specific gravity compare to other conducting polymers
concentration. The sensor has a recognition component that like: polypyrrole, polyacetylene, polythiophene ect. and
acknowledge to a particular group of analytes. Another main polyaniline is most biocompatible material [11]. Polyaniline
component of biosensor is transducer or detector electrodes, (PANI) exists in different structures forms as per chemically
which is complexes with analytes, called Bioreceptor [2]. and physically. These localized states are: Leucoemeraldine
(C6H6NH)n, Emeraldine(Green for emeraldine salt and blue
The glucose biosensor is based on the nature of for emeraldine base).Among structures most mutual is
bio-recognition which is called bio catalytic device. A greenish protonated polyaniline (emeraldine salt most
bio-catalytic device allows enzymes, cells, and group of cells conductive) has higher conductivity compare to the,
i.e. tissues. This recognises the target analytes. Conducting polyaniline (emeraldine base i.e. non conductive) in bluish
polymer polyaniline (PANI) and its group of surfactants are colour and per nigraniline blue violet colour [12].

Aniline (Molecular wt. 93) is colourless liquid, which

Manuscript received April 28, 2014.
Shatrudhan Palsaniya, Veerender Sharma, Centre for Materials Science
gradually turns yellow or brown. It soluble in organic
and Engineering, National Institute of Technology, Hamirpur H.P. compound and water [13]. Aniline in solution adsorbs
India,177005 strongly to colloidal organic materials, which raises its
Veerender Sharma, Centre for Materials Science and Engineering,
National Institute of Technology, Hamirpur H.P. India,177005
solubility and dynamic movement of nanoparticles in to
prescribed solution [14]. Adsorption depends upon pH of

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 Synthesis of nano structured polyaniline with ionic and nonionic polymers based enzymatic application of glucose
biosensing

solution [15]. The presence of surfactant increases the ability was shows higher amperometric current so we refers
of conductivity but reduced the electrical stability of PANI-SDS-F123 at nano structure level. Because
polyaniline because polyaniline has high surface area which transferring of electron is higher in this material so it w
entrapped by surfactant and affects the electrical stability shows higher response .We has various characterizations up
[16-17]. Surfactants are main gradient component in to nano level.
polymerization of aniline to enhance the property of
polymers with respect to conductivity, solubility in to the
organic solvents [16]. II. MATERIALS AND METHODS
There are different-different methods for polymerization of
monomers like: A. Materals used in synthesis
Seeding polymerization, templets methods, electrochemical Chemical used in above references to synthesis the PANI
synthesis, and vibrational irradiation. In these methods nano-structrued particles with the various compositions as
important term is organic acids which forms micelles upon above defined. In this way we have to use following
the aniline, after polymerized .In this case micro level materials:
clusters are formed like nano fibers [18]. Surfactant increases Aniline monomer in liquid form as light yellow or brown
the diameter of the nanostructure particles [19]. Polyaniline colours which stored in dark place. Hydrogen Peroxide
makes a aques interface with nano surfactant entrapped (30%) GR ,H2O2 ,Mol. Wt. is 34.01 g per mol. HCL and
fibers, which was generated from surfactant and co-dissolved Sodium dodecylsulfate (SDS).Polyoxyethylene lauryl ether
in to the solution. This technique is called interfacial called Brij 35 Mol. Wt.1199.56 purchased from ACROS
polymerization [16-19]. At this level, after interfacial Organics. Sodium phosphate dia basic AR (Anhydrous)
polymerization we have to dissolve the Ammonium per Mol. Wt. 141.96 (Na2HPO4), Ammonium per sulphate
Sulfate (APS).in deionized water for aques solution. In this (APS), 98% ACS reagent, Mol.wt. 228.19 gm per mol,
method the genesis of nano fibers become very low quantity, H8N2O8S2, Glutaraldehyde (25% aques solution C5H8O2,
because they get oxidized [20]. Mol.wt. 100.12 gm per mol), Pluronic F123, polyethylene
Polyaniline prepared using soft template method as well as glycol (PEG) Mol.wt. is 4000 gm per mol., Glucose Oxidase
hard template methods. Soft template method based (Gox Type 2-s Aspergillus niger),Pluronic F123 it is a
materials can be easily washed and prepared. But hard polymeric nonionic reagent, Deionized water from Bio-age
template based materials we have to use external catalyst like system at resistivity 18.3 M per cm was used in all cases to
metallic materials to enhance the rate of reaction [21]. The prepare aques and chemical molar solutions, purchased
effective method to raise the surface to volume to ratio is to from SIGMA ALDRICH.
induct mesophase by using wetting agent, which form a super
molecule gathering [22]. The mixed surface active agent is B. Synthesis methods of nanoparticles
better method to ascendance the sizing of nanoparticles over
wetting agent /coemulsion [23].The particle emergence in
The mainstream PANI and its various compounds are
mixed microemulsion arrangement is quick complicated,
synthesized using ionic and non-ionic polymeric surfactant
which affects directly the size of particle and surface activity
as a structure directing agent, for example sodium dodecyl
[24].Conducting polymers shows qualitative response as
sulphate, dodecyl benzene sulphonate (SDBS) and camphor
sensor for functional group like: alcohol evaporation such as
sulphonic sulphate. Below given table shows the various
alkenols [24-25]. Polyaniline (PANI) and its alternative
chemical compositions as concentration variation activity.
derived function such as
poly(o-toluidine),poly(o-anisidine),poly(N-methylaniline),p Aniline SDS Relati
oly(o-N-Ethylaniline),poly(2,3-dimethylaniline)and Chemical
Concen Concen Pluroni pH ve
poly(diphenylamine) were found sensitive to alkanol [26]. Compositi
To find out the concentration of glucose in our body system as tration tration c F123 value Visco
on
well as in several aspects like nutrient, micro-organism and (M) gm (M) gm sity
in the field of aesulapian/medicine [27-28]. The invention of PANI-SDS 1.8 gm 3.0 gm - 0.816 1.16
glucose biosensor is crucial due to preponderance of heart
PANI-SDS
valves diseases is an important threat. There are several 2.0 gm 3.0 gm 1.5 gm 0.579 1.01
methods to methods to recognize glucose like: -F123(a)
electrochemiluminisence, capacitive detection, fluorescence PANI-SDS
2.5 gm 3.0 gm 1.5 gm 0.52 1.03
detection, but highly efficient in form of current -F123(b)
amperometry is best to determine to the glucose [29].Now I PANI-SDS
have to describe that there are methods to find out the 1.8 gm 3.0 gm 2.0 gm 0.67 1.41
-F123(c)
mesostructured PANI at nanostructure level .we have used
PANI-SDS
ionic materials like sodium dodecylsulfate as surfactant 1.8 gm 3.0 gm 2.5 gm 0.84 1.71
-F123(d)
containing as self mixed property in form of mesostructured.
Again there is non-ionic surfactant polymer as Pluronic
-F123 (EO20PO70EO20), Brij-35(Polyoxyethylene lauryl Now we have to describe solution PANI-SDS and for
ether).Among the surfactant when we made the following remaining all solutions procedure are same. Take the
materials like: PANI-SDS-F123, PANI-SDS, and commercially available 12M HCL; dissolve 1.5 gm in 120
PANI-SDS-Brij-35 among the materials PANI-SDS-F123 ml deionized water and make aques solution of it. Now take

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 International Journal of Engineering and Technical Research (IJETR)
ISSN: 2321-0869, Volume-2, Issue-5, May 2014
2.0 gm aniline monomer in liquid form and dissolved in to III. CHARACTERIZATION OF MATERIALS
40 ml aques solution of HCL and stirrer up to 1 hr. Now take
3.0 gm ionic polymeric surfactant sodium dodecyl sulphate A. X-Ray diffraction pattern
(SDS) and mixed in to the remaining in 80 ml aques solution
of HCL and stirrer up to 1 hr for completely polymerization Materials characterizations recorded using material
of aniline and becomes homogeneous solution. In this analytical equipments like X Ray Diffraction (X-RD), PAN
manner surfactant get started micelles formation and air get Analytical expert PRO Diffractometer using Cu K
entrapped by surfactant and aniline starts polymerization .It radiation (=0.1541 nm,40 kv,21 mA). The detector moved
remains stable form due to structure directing agent SDS step by step from 4 to at the speed of 2 /min.ad X-ray
and reduce the size of nano-surfactant. powder placed under 40 kW at 21mA.
Now we have to make a provision of temperature for The X-Ray diffraction model of polyaniline at various
oxidation at 0-3 degree centigrade, using ice tub and keep concentrations were represented in Fig.as expressed
PANI solution in it and start to stirrer. In this way to make in elemental analysis. The characteristics design graph of
conductive materials this solution we have to employ under organic compound which doped in polyaniline has been
oxidation reaction after mixing ammonium per sulphate obtained some different but not more different. All of the
(mixed APS 9.0 gm in deionized water and make aques profile were same but differ in corresponding intensities
solution ammonium per sulphate). Dissolving of APS peaks [30]. There are two types of angles in X-RD pattern,
should be slowly in surfactant solution. APS reduces the wide as well as low angle [31-32]. The wide angle is
concentration of surfactant in form of oxidation and attribute continues along to the polymer long chain 2 =...
enhances the conductivity of green emeraldine base. This while the maximum peak where the centered peak was 2 =
solution has to remain static up to 3 days. In this way
which causes by continuously perpendicular to
prepared solution is PANI-SDS emeraldine base Now
the polymer chain [31]. Low angle area graph is measured in
similarly we ca make solution of PANI-SDS-F123 (a) in
the range of to 5 .We know that polyaniline is porous in
non-ionic polymeric surfactant. For this we have to proceed
as following manner: nature so X-RD shows its nature not a sharp peaks but a
Prepare 1.5 gm, 12 M commercially available HCL solution curvature type graph smoothly lines we get which clearly
in 120 ml deionized water, from which 40 ml solution stirrer shows that resultant material is polymer. Materials which
up to 1 hr with 2.0 gm aniline monomer. Prepare a are mixed with highly polymeric materials
homogeneous solution of SDS and F-123 for this we have to (PANI-SDS-F123) like F-123 surfactant, this covers large
use, 3.0 gm SDS and 1.5 gm Pluronic F-123 and stirred up surface to volume ratio, so in this case low as well as wide
to 0.5 hr up to complete polymerization and become angle were calculated. But in case of with out polymeric
completely dissolved. After complete polymerization we materials (PANI-SDS) there is not possible to calculate the
have to mixed oxidizing agent APS drop wise slowly (APS low angle.
solution prepare using 100 ml deionized water stirred with
9.0 gm APS). This whole arrangement should be at 0 degree B. Fourier Transform Infrared Radiation Spectrum
to 4 degree centigrade temperature. After complete mixing
of APS we have to leave this solution static up to 3 days at 4 In general principles of Infrared spectroscopy including
to 5 degree centigrade temperature. In this way it will fourier transform infrared spectroscopy (FTIR) technique
completely polymerized and become dark greenish colour. measure the absorption of radiation by high frequency (i.e.
This solution does filter and dry in vacuum oven for 48 hr at optical branch) phonon vibrations and they are also sensitive
40 degree centigrade temperature. to the presence of particular chemical groups such as
hydroxyl (-OH),Methyl (-CH3),Imido(-NH),and
C. Activity of nano particles Amido(-NH2),Each of these groups absorbs infrared
radiation at a characteristics frequency and the actual
I this way we have prepared different composition in fixed frequency of absorption varies somewhat with the
proportion and molar ratio. When we increase the environment .We discuss some result based on work of FTIR
concentration of aniline than resultant solution become dark ,PerkinElmer ,Spectrum65,Model no.SP-65 [33].
greenish colour, and when increases the concentration of
Pluronic F-123 then solution turned in greenish colour with
nano fibers.
When concentrations of non-ionic polymeric surfactant
increases then small nano structured fibers are arises. But at
lower concentration of Pluronic F123 these are completely
oxidized b APS and gives fine dark greenish powder after
dry. This powder get illumination under sun light , because
conductive nano particles when gets start to scattering
motion then an energy is liberated and they gets illuminated.
Every scattered particle are arranged in symmetrically and
shows elastic motion. So in case of conductivity what is
nearly band edge absorption after UV Visible spectroscopy Fig: (1) FTIR spectra of PANI-SDS-F123 samples and
can be determine most probable band gap. study.

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 Synthesis of nano structured polyaniline with ionic and nonionic polymers based enzymatic application of glucose
biosensing

FTIR spectra of conventional PANI and its samples with The exact wave number at 1220 cm-1 shows C-N stretching
different concentrations have been shown in above of benzene ring. There are three peaks of C-N group
spectrum. Fig: 1 shows the polymeric compound of matching in which one is sharp and one is round shape at
PANI-SDS-F123 with different concentration of F123 from exact 1220 cm-1 wave number. These indicate that mixed
1.5wt% for spectrum S1, 2.0 wt% for spectrum S2 and compositions like polymeric surfactant F123 mixed in varies
2.5wt% for spectrum S3 and spectrum S4 for PANI. Above concentration increases sharpness in spectrum because of
spectrum shows bond stretching at various peaks of nature of emeraldine base increases [35]. The range from
spectrum. These peaks show differentdifferent 743 to 813 cm-1 shows mixed doping of the moiety
compositions at varies concentrations of polymeric compounds like high surface area directing agent SDS and
surfactant in Fig 1 (a). It shows that high bond energy in F123,and make a dark greenish salt in meso structured form.
C-C shows at wave number of 1462 cm -1 to 1545cm-1 and All samples were in emeraldine oxidation state and conform
C=C stretching at approximate 1500cm -1.This stretching of that pure greenish after stabilized polymerization and
bonds and vibrations on benzene ring and its conjugate purplish colour before oxidation starts [36]. Some peaks are
elements gets vibration of quinoid ring and benzene ring. more sharp means highly intense at 1500cm -1 and
This shows the emeraldine salt (ES) of 2900cm-1.It means a complete polymerization with regular
polyaniline.PANI-SDS-F123 shows C-C stretching overall arrangement of polymerized material which have high
ranging 1500cm-1 to 1545cm-1 for (ES) emeraldine salt Fig: energy in form of absorbance that shows highly intense peak
1. Except that remaining peaks came on different wave [37].
numbers. The absorptions at alternate wave number like The compound materials PANI-SDS-F123 is compared with
1220,1500,1462,1063cm-1[34].Fig 2 shows more the standard PANI and surfactant SDS, stretching of sulfate
concentration of aniline monomer with structure direct ion with S=O is 1213-1232 cm-1 standard. But in this case
agent (SDA) compound is PANI-SDS.The peak at 1225cm-1 here 1218 cm-1 showing peak is S=O sulfonate stretch. In
show C-N stretching more absorbance compare to case of SDS there are CH- ,-O-CH2- and O-SO3- bonds
PANI-SDS-F123 polymer. are available so every bond has specific peak and bond
stretching respectively. Here some peaks are highly sharp
which shows that corresponding intensity of the functional
500 1000 1500 2000 2500 3000 group. In case of aeromatic compound meta CH- strongly
S9 stretching shows at 809 to 818 cm-1 and CH- band para
shows at 850 cm-1.-SO- stretching shows at Fig: 2 spectrums
S8 S9 at 809 to 1069cm-1. In the sample S6 and
S7concentration of F123 increases the CH- started to show
S7
weakly stretching at 2850 cm-1 and at reducing the
S6
concentration of F123 it started to show CH- stretching at
2950 cm-1. Again we can say that to increase the
Transmittance

concentration of aniline monomer it started to stretch at

S5
various points like Ortho, Meta and para of the CH- and
S4 NH- groups. At 2950-3100 cm-1-NH- shows the primary
absorption because PANI (6:1) S9 due to high concentration
S3
of aniline monomer CH- strongly stretch i.e. completely
disappeared. This is the reason that a sharp comes at
2850-2900 cm-1. Here all vibrational frequencies have been
S2

S1
shows of exact composition of PANI-SDS-F123 materials.

500 1000 1500 2000 2500 3000

Wavenumber(cm )
-1
C. UV-VIS Absorption spectrum

UV-VIS absorption spectrum mainly used to identify to the

Fig (2) FTIR spectra of PANI-SDS-F123 with PANI and SDS band edge absorbance. The instrument is PERKIN ELMER
Lantrisant, CF728YW UK LAMBDA 750 Part no.
S1 --- PANI-SDS L6020041.Polyaniline haves - electronic transition in to
S2 1:0.2 PANI-SDS-F123 benzenoid segment and bond also. In PANI conductivity
S3 1:0.6 PANI-SDS-F123 mainly causes via electronic cloud. So at this level
S4 1:0.7 PANI-SDS-F123 first absorbance band comes by benzenoid segment and
S5 1:0.9 PANI-SDS-F123 other two are due to dominating part like F123 concentration
S6 1:1 PANI-SDS-F123 and formation of corresponding polaron at polyaniline after
polymerization [39]. Different concentration containing
S7 1:3 PANI-SDS-F123
PANI-SDS-F123 shows characteristics absorbance at
S8 1:4 PANI-SDS-F123
400-441,600-640,721-841nm wavelengths. As the
S9 6:1 PANI-SDS-F123 concentration of monomer increases corresponding peak

32 www.erpublication.org
 International Journal of Engineering and Technical Research (IJETR)
ISSN: 2321-0869, Volume-2, Issue-5, May 2014
increases, maximum peak gets at 841nm and minimum peak
gets at 400 nm.
The overall specturm not long falling,because absorption
specturm showing that received peaks are shifted from 40
nm wavelength. This shifteing of wavelength is due to band
locating of the polaron aroungd the 721-841 nm. At this
range shows the formation of band polaron due to
F123.PANI shows shifting due to small surfactant SDS
micellers at 400-441 and 600-640 nm. After finding the
absorption of particular functional group at specific
wavelength.In this way we can find out band edge of our
semiconductor materials.Band edge depends on the
absorption cofficient () and related energy (h)2 of the
materials i.e. absorbed [38].
PANI-SDS-F123 (1:0.5)

400 500 600 700 800

1.7
1.6 PANI-SDS-F123 (1:1)
1.5
1.4
1.3
1.2
1.5
1.4 PANI-SDS-F123 (1:3)

1.3
1.2
1.1
1.3 PANI-SDS-F123 (1:1.5)

1.2
Wavelength

1.1

1.4
1.0
1.3 PANI-SDS-F123 (1:0.8)
1.2
1.1
1.0
0.9
1.3
1.2
PANI-SDS-F123 (5:3)
1.1
1.0
PANI-SDS-F123 (1:0.6)
0.9
0.8
0.7
1.2
PANI-SDS-F123 (1:0.5)
1.0

0.8

0.6
400 500 600 700 800

Absorbance

Fig (3) UV Vis absorption spectra for PANI-SDS-F123

synthesized at different aniline and F123 concentrations

D. Scanning Electron Microscopy (SEM) Images

At various concentrations PANI-SDS-F123 materials have
been prepared and corresponding SEM images also we have PANI-SDS-F123 (1:0.8)
get. The low concentration of SDS as micelle directing agent
which polymerized aniline in to nano rods of PANI.

PANI-SDS-F123 (1:1.5)

PANI-SDS

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 Synthesis of nano structured polyaniline with ionic and nonionic polymers based enzymatic application of glucose
biosensing

measurement provides some parameter like, capacitance(C),

dissipation factor (D), resistance(R).

Ac conducvtity

0.025

0.02

0.015

Ac conducvtity
0.01

PANI-SDS-F123 (1:3)
0.005
Here ratio of sodium dodecyl sulfate (SDS) materials is kept
constant through out chemical synthesis of PANI.Where as 1000 10000 100000 1000000 1E7

the changing the concentration of the surfactant (SDS) and Frequency

co-polymer surfactant F123 in fixed proportion respectively.
Here showing SEM images are porous and rod type in
nature. This is suitable for involving of enzyme. The porous
matrix increases sensitivity of glucose biosensor. So it can Fig 5 A.C. conductivity changes with the frequency at log
enclose the Bioreceptor with enzyme easily for longer time. scale
The scanning electron microscopy (SEM) pictured
above.SEM model no. i.e. FEI-QUANTA 450 FES we have
The a.c. conductivity we have found out using a
used. All pictures bearing the PANI nanofibers and particles
relation of under following [42].
at micro level. Above pictures shows uniform distribution of
PANI particles where shapes like small leaves. The small
nano fibers with 3 m and some nano fibers 2.5m
total () =ac () + dc () (1)
diameters. The 1:3 proportion haves 500 nm diameter of
Where ac () = 2f 0 tan () . (2)
nano dendrites. Upper age of size of PANI respond to
~200-500 nm diameters of nanoparticles and length between
Here tan () = loss factor
the two dendrites is 1-3 m. At higher magnifications, the
Cp = Capacitance factor
resolution of image is distorted in last image. It means
f= Alternating current frequency
further we cant resolve to this picture. Here various
0=Permittivity of free space
concentrations varies composition has prepared. So
according to change of concentration of monomers as well as
We have made a small spherical pallet using palletization
surfactant and co-surfactant than affected structure and size
pressing machine at 150 lb pressure. This pallet has 13.12
of nanofibers. As per concentration of co-surfactant are
mm diameter (D) and thickness (d) is 1.60 mm. Here total
increases then agglomerate started of PANI and its
conductivity is a.c. as well as d.c. In this case
compositional materials. This effect we can see in 1:0.5 to
d.c.conductivity is not considered due to a.c. frequency
1:3 proportion type SEM images [40].
dependent measurement. So a.c. conductivity we have
obtained using dielectric constant i.e. .

E. A.C. Conductivity Measurement

Where = (Cp d) / (0 A) ... (3)
The electrical conductivity measurement of And Area of pallet is = so from here = 11.84

PANI-SDS-F123 composite material is measured using the

LCR meter model no. WAYNE KERR 6520 A [41]. The
frequency range of this instrument is 100 Hz-15 MHzs
In this way we have find out overall a.c. conductivity and
During measurement of a.c. conductivity we have find that
drawn graph in origin then we see that above 1MHz
increasing order of the conductivity with frequency i.e. .
frequency highly increasing the conductivity. Similarly we
There are polaron, bi-polaron, solitons are moves in overall
can draw the relation between dielectric constant and
materials surface structure in chain formation so that this
frequency. Which shows that decreases w.r.t. the applied
phenomenon creates a conductivity at the frequency. So
frequency.
electrical conductivity ac of PANI-SDS-F123 composite
shows higher response beyond 1MHz [42].This

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 International Journal of Engineering and Technical Research (IJETR)
ISSN: 2321-0869, Volume-2, Issue-5, May 2014
E' electrode. In this procedure the sensing study of H2O2 was
120 performed using PANI-SDS-F123 samples. This result
shows that PANI-SDS-F123 electrode on successive
100
addition of H2O2 in to 0.1 M Phosphate buffer solution
(PBS) (pH~7.0) exhibits higher current than PANI for same
concentration of H2O2 as shown in fig7 below.
80
E'

A 1mM H2o2
60
B 5 mM H2o2
0.0003
C 10 mM H2o2 B
C
40
0.0002

Current (Amp)
20 0.0001 A
100000 200000 300000 400000 500000 600000 700000 800000

Frequency
0.0000

D-Factor
-0.0001

0.0 0.2 0.4 0.6 0.8

250
Potential i(Volt)

200
Fig: 7 Cyclic Voltammogram of PANI-SDS-F123
150
D-Factor

100

50

100000 1000000 1E7

Frequency

Fig 6 Changes of dielectric constant and loss factor w.r.t.

a.c. frequency at room temperature
As the doping gradient is increases then conductivity is
increases up a finite level [43]. But concentration of
monomer is increases then conductivity is decreases in case
of glucose sensing. Because polymerized particles are inter
cross linked and agglomerate on the surface of secondary Fig: 8 CVs of planer Pt/PANI-SDS-F123/GOx immobilized
surfactant like F123. Due to this reason the transferring of electrodes
conjugated ions decreases and conductivity decreases. But at
1:1 ratio of Aniline: F123 shows higher conductivity. Here PANI-SDS-F123 shows electrocatalytic ability in the
showing characterization of loss factor and relative reduction and oxidation of H2O2 in various concentrations
dielectric constant w.r.t. frequency. In both cases and of H2O2 PBS solution [45].
tan() decreases as the frequency increases. Fig 5 shows
sudden increases in conductivity. So such type of materials b) CV response with Glucose concentration
can be employed in electrical and electronic application like,
micro-strip antennas and in solid state devices. Cyclic voltammetry measurements were performed in a
three electrode system. The working electrode is Pt disk is
fabricated with polymeric materials and counter electrode is
Pt. foil and reference electrode is Ag/AgCl/KCl salt.
F. Glucose Sensing Characteristics Potential scanned from -0.2-1.0 V with scan rate of
Amperometric, cyclic voltammeter (CV) measurement has 50mV/sec. All three electrodes were to a common
to perform using (CH-Instrument, USA) in a conventional potentiostat that control that controls the impedance
three electrode cell [44]. measurements and immersed in to a conducting solution
such as PBS. Fig 8 shows cyclic voltammogram (CVs) of a
planer Pt/PANI-SDS-F123/GOx fabricated electrodes in the
a) CV Characteristics with H2O2 presence of (enzyme) glucose oxidase. As shown in fig 8 the
electrode current in the presence (40mM) of GOx is less than
H2O2 sensing and glucose sensing was performed using CV the current in the absence (0 mM) of GOx. In the case of
and continuous amperometry. The electrochemical cell was GOx immobilization, the current of the CV is decreased in
formed by a three electrode arrangement using Ag/AgCl as the absence of the substrate, because of surface of the
the referenced electrode (KCl salt bridge), polymer coated electrode is covered by GOx [46].
on Pt disk as the working electrode and Pt foil as the counter

35 www.erpublication.org
 Synthesis of nano structured polyaniline with ionic and nonionic polymers based enzymatic application of glucose
biosensing

G. Amperometry H2O2 sensing solution at 25 second interval. At last we obtained a linear

Same quantity of PANI-SDS-F123 i.e. used in CV step sized curved means as concentration added then
proceeded in following manner. oxidation reaction takes place and current rises up to fixed
amplitude and after that it remains constant up to complete
C
oxidation. It means current response is based on the
10 formation of H2O2 during the oxidation reaction at
9 PANI-SDS-F123 and GODx immobilized electrodes .The
8
electrode oxidation reaction as followed reaction [47].

7
CURRENT in

6 WE(1).Current (A)
0.0018

5
0.0016

4 0.0014

3 0.0012

2 0.0010

Current (Amp)
0 50 100 150 200 250 300
0.0008
TIME(sec)

0.0006

0.0004

Fig: 9 Amperometric response of H2O2

0.0002

0.0000

A 0 100 200 300 400 500

12 Linear Fit of A Time (Sec)

11
1mM H2O2 added at every 20 second

10 Fig: 11 Amperometric Response of Glucose Concentration

9
Current( cm )

8
2

A
7
12 Linear Fit of A
6
11
5
10
4
9
3
Current( cm )

8
2

7
1
0 5 10 15 20 25 30 35 40 45 50
6
Glucose Concentration(mM)
5

Fig: 10 Calibration curve of H2O2 sensing of electrodes 4

2
Amperometric response of the PANI-SDS-F123 and
1
fabricated electrodes from polymer of successive addition of 0 5 10 15 20 25 30 35 40 45 50

H2O2 and calibration curve for the biosensor response to Glucose Concentration(mM)

H2O2 has shows in above figure 9.As per H2O2 added the
response of sensing is step wise increasing in reverse order. It Fig 12 Calibration curves of enzyme electrodes for glucose
doesnt matter that calibration curve remains in forward
order or reverse order beside the step function is increasing D-Glucose + O2 GOx Gluconic acid + H2O2
order. H2O2 O2 + 2H+ + 2e-
Ag/AgCl Standards KCl and
GODx represents enzyme Glucose Oxidase in oxidized state
H. Amperometry glucose Sensing and reduced state of enzyme, respectively. The reoxidize
current of H2O2 is detected at the electrode in order to
The current measurements are does by the Amperometric determine the glucose concentration. It exhibits a good
measurements. This technique is based on the current linearity for sensing glucose in the range 1 mM to 45 mM.
response means oxidation reaction of analytes and time in
seconds. It means Amperometric response is based on the a) Amperometric Linear Response
current and time characteristics. In experimental part we Amperometric response obtained from the figure 10, from
have to prepare a D-glucose (Grape Sugar) solution and keep which it is clearly seen that the enzyme electrode produces a
it stable up to 24 hr. After that this solution employed under linear steady state amperometric response up to 50 mM
PANI-SDS-F123 and Glucose Oxidase fabricated electrodes successive addition of glucose concentration [48]. The
at fixed applied potential. Characteristics of current versus existence of this linear relationship between the current and
time obtained a linear step function. During measurement concentration of glucose is important for the accurate
we have to added 1mM glucose concentration in to the determination of glucose levels

36 www.erpublication.org
 International Journal of Engineering and Technical Research (IJETR)
ISSN: 2321-0869, Volume-2, Issue-5, May 2014
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