A student presented their work on cyclic voltammetry. They prepared a 2mM potassium ferricyanide solution with 1M KNO3 as the supporting electrolyte. They polished a platinum working electrode and performed cyclic voltammetry under nitrogen purge. The resulting cyclic voltammogram showed a cathodic peak when Fe(CN)6^3- was reduced and an anodic peak when Fe(CN)6^4- was reoxidized. Analysis of the voltammogram provided information about the redox reaction such as peak potentials and currents. The student demonstrated the experimental procedure for cyclic voltammetry.

1. Presented by:
 MONALIN MISHRA
 Registration No.- 1412106023
 Integrated MSc. in Applied Chemistry
 College of Engineering and Technology (CET), BBSR
1

2. 2
Little Pre-requisite Knowledge
What is needed to run the experiment?
Experimental Procedure
Applications
Why CV?
Conclusion
My work Plan
Bibliography
Acknowledgement

3. 3

4. 4
 Electrochemistry is the branch of chemistry which is
concerned with the interrelation of electrical and
chemical effects.
 It basically involves chemical phenomena associated with
charge separation which often leads to charge transfer
on electrode surfaces.
 The two basic electrochemical cells involved in these
analyses are Galvanic and Electrolytic cells.
ELECTROCHEMISTRY:

5. ELECTRO ANALYTICAL TECHNIQUES:
Electro analytical chemistry involves the analysis of
chemical species through the use of electrochemical
methods.
Generally, alterations in the concentration of a chemical
species by measuring changes in current in response to
an applied voltage is monitored with respect to time.
5

6. 6

7. 7
Voltammetry
Cyclic
Voltammetry

8. 8
 Faraday's laws of electrolysis are quantitative relationships
based on the electrochemical researches published by Michael
Faraday in 1834.
FARADAY’S LAW OF ELECTROLYSIS:
 Faraday’s 1st Law Of Electrolysis:
The amount of chemical reaction which
occurs at any electrode during electrolysis by a current
is proportional to the quantity of electricity passed
through the electrolyte. Mathematically,
M or W = Z.I.t =ZQ
W or M = Amount of substance liberated in gram
Q = Quantity of electricity passed in coulomb
I = Current in ampere
t = Time in seconds
Z = Proportionality constant called electrochemical equivalent

9. 9
 Faraday’s Second Law Of Electrolysis:
The amounts of different substances
liberated by the same quantity of electricity passing
through the electrolytic solution are proportional to
their chemical equivalent weights (Atomic Mass of
Metal ÷ Number of electrons required to reduce the
cations). Mathematically:
Amount deposited (gm) = m x Q
F x n
m = atomic mass of substance
Q = Total electric charge passed through substance
F = Faraday’s Constant
n = electrons transferred per ion

10. 10
The Transport Mechanism:
The current generated by the oxidation and reduction of
some chemical substance at the electrode i.e., the faradic
current that flows at any time is a direct measure of the
rate of electrochemical reaction taking place at the
electrode.
Further, the current itself is dependent upon two things-
1) The rate at which electron can transfer across the
interface called the charge transfer.
2)The rate at which material gets from the bulk of the
solution to the electrode called the mass transport.

11. 11
(i) diffusion – motion of a
species caused by a concentration
gradient.
(ii) migration – movement of
ions through solution by electrostatic
attraction to charged electrode.
(iii) convection – mechanical
motion of the solution as a result of
stirring or flow.
Three mass transport mechanisms:

12. 12
The mechanism of electron transfer at an
electrode:
The mechanism consists of the following steps-
1. Diffusion of the species to where the reaction occurs.
2. Rearrangement of the ionic atmosphere.
3. Reorientation of the solvent dipoles.
4. Alterations in the distances between the central ion
and the ligands.
5. Electron transfer.
6. Relaxation in the inverse sense.

13. 13
VOLTAMMETRY:-Electrochemical method in which information
about an analyte is obtained by measuring current (i) as a function
of applied potential (V).
INSTRUMENTATION - Three electrodes in
solution containing analyte.
Working electrode : microelectrode whose
potential is varied with time.
Reference electrode : potential remains constant.
(Ag/AgCl electrode or calomel)
Counter electrode : Hg or Pt that completes
circuit, conducts e- from signal source
through solution to the working
electrode.
Supporting electrolyte : excess of nonreactive
electrolyte (alkali metal) to conduct
current.

14. 14
Voltammetry is Different from Other Electrochemical
Methods:
a) Potentiometry: measure potential of sample
or system at or near zero current.
voltammetry – measure current as a change
in potential.
b) Coulometry: use up all of analyte in process
of measurement at fixed current or potential.
voltammetry – use only small amount of
analyte while varying potential.

15. Different types of voltammetry:
Squarewave Voltammetry (SWV)
Anodic Stripping Voltammetry
Cathodic Stripping Voltammetry
Adsorptive Stripping Voltammetry
Alternating Current Voltammetry
Normal Pulse Voltammetry
Chronoamperometry
Staircase Voltammetry
Differential Pulse Voltammetry
Polarography
Linear – Sweep voltammetry
Cyclic Voltammetry (CV)
15

16. Linear sweep voltammetry (LSV): The current at a working
electrode is measured while the potential between the working
electrode and a reference is swept linearly in time.
Cyclic voltammetry: The same as LSV but the potential is swept
in a way that the experiment ends where it started.
16

17. 17
Cyclic voltammetry (CV) is a powerful and
popular electrochemical technique commonly
employed to investigate the reduction and
oxidation processes of molecular species.

18. 18

19.  Cyclic voltammetry (CV) is the
most frequently used technique
for acquiring qualitative
information about electrochemical
reactions.
 Almost any electrochemical study
starts with application of CV.
-0.04
-0.03
-0.02
-0.01
0
0.01
0.02
0.03
0.04
0.05
-0.4 -0.2 0 0.2 0.4
19
 The power of cyclic voltammetry results from its
ability to rapidly provide considerable information on
the thermodynamics of the redox processes and the
kinetics of heterogeneous electron transfer reactions
and on coupled chemical reactions or adsorption
process.

20. 20
This technique is based on varying the applied potential
at a working electrode (compared to the reference
electrode) in both forward and reverse directions while
monitoring the current between the auxiliary electrode
and reference electrode

21. Potential
time
21
Variation of the applied potential as a function of
time in a cyclic voltammetry experiment:
Forward
scan
R everse
scan

22. 22
Cyclic Voltammogram

23. 23
The important parameters are:
the initial potential, Ei
the initial sweep direction
the sweep rate, v
the maximum potential, Emax
the minimum potential, Emin
the anodic peak current, ipa
the cathodic peak current, ipc
the final potential, Ef

24. 24
+1.0 V -1.0 V
Emax
Emin
+ current, cathodic
- Current, anodic
ic
ia
E1/2
+V -V
ipc
ipa

25. 25
 For a reversible reaction, the peak current for the
forward sweep of the first cycle is proportional to the
concentration of the analyte and the square root of
the sweep rate (Randles–Sevcik expression):
 n is the number of electrons in the half-reaction
 A is the area of the electrode
 C is the concentration of the analyte
 D is the diffusion coefficient of the analyte
 v is the sweep rate
 From this equation, it can be concluded that the peak
current increases with the sweep rate, with the
concentration and the area of the electrode as long as
the reaction is reversible.
2/12/12/35
*****)10*69.2( vDCAnI 

26. 26
Volta
Voltammogram of a bare electrode under Nitrogen.
Voltammogram of a bare electrode under air.
Voltammogram of a complex under nitrogen.
Voltammogram of a complex under air.

27. 27

28. 28
 At 25 0C (298 K) the Nernst Equation is simplified
this way:
NERNST EQUATION:
E(cell) = E0
(cell) – RT/ n F ln [Ox]
[Red]
 The Nernst equation relates to the activities of the
species involved with the electrode potential (E) of
the half-reaction and its standard electrode potential
(E0) which is the value of the potential relative to
the standard hydrogen electrode when the activities of
all species are unity.
Where, F = Faraday constant
R = Gas Constant
T = Temperature

29. 29
 The characteristic peaks of cyclic voltammogram are
caused by the formation of the diffusion layer at the
electrode surface.
 This can be best understood by carefully examining
the concentration ~ distance profiles during the
potential sweep.
 The continuous change in the surface concentration is
coupled with an expansion of the diffusion layer
thickness.

30. 30

31. 31

32. 32

33. 33
The working electrode carries out the electrochemical event of
interest.
The most important aspect of the working electrode is that it
is composed of redox inert material in the potential range of
interest.
It must be an electrical conductor as a working electrode acts as
a source or sink of electrons for the exchange with molecules in
the interfacial region where the solution is just adjacent to the
electrode surface.
It must also be electrochemically inert i.e., it does not generate
a current in response to an applied potential over a wide
potential range (the potential window).
 The type of working electrode can be varied from experiment
to experiment to provide different potential windows
WORKING ELECTRODE:

34. 34
Commonly used working electrode materials for
cyclic voltammetry include platinum, gold,
mercury, and glassy carbon.
Other materials (e.g., semiconductors and other
metals) are also used, for more specific
applications.

35. 35
Reference Electrodes
A reference electrode has a well defined and stable
equilibrium potential.
It is used as a reference point against which the
potential of other electrode scan be measured in an
electrochemical cell.
Normally a standard electrode is used whose potential
is constant throughout the experiment.

36. 36
The most commonly used reference electrodes for
aqueous solutions are the calomel electrode and
the silver/silver chloride electrode (Ag/AgCl).
Electrodes are commercially available in a variety
of sizes and shapes.

37. 37
The auxiliary electrode is typically a platinum wire that
provides a surface for a redox reaction to balance the
one occurring at the surface of the working electrode.
It does not need special care, such as polishing.
In order to support the current generated at the
working electrode, the surface area of the auxiliary
electrode must be equal to or larger than that of the
working electrode.
Some common reference electrodes used in aqueous
media include the saturated calomel electrode (SCE),
standard hydrogen electrode (SHE), and the Ag/AgCl
electrode.
AUXILIARY ELECTRODE:

38. 38
Workin g E lectrode.Counter Electrode. Reference Electrode

39. 39
The medium required for electrochemical experiment
must be conducting which can be achieved by using an
electrolyte solution.
An electrolyte solution is made by adding an ionic salt
to an appropriate solvent.
The mixture of the solvent and supporting electrolyte
is commonly termed the “electrolyte solution”.
The salt must become fully dissociated in the solvent in
order to generate a conducting (i.e., ionic) solution.
The electrolyte solution must also be able to dissolve
the analyte, must be electrochemically inert over a wide
potential range (i.e., no current due to electrolyte
solution oxidation/reduction), and must be pure (e.g.,
the presence of water decreases the size of the
potential range).
ELECTROLYTE SOLUTIONS:

40. 40
It must also be chemically inert, so that it will not
react with any reactive species generated in the
experiment.
If the temperature is to be varied, the electrolyte
solution must have an appropriate liquid range.
Electrolyte solutions can be aqueous or non-aqueous.

41. 41
Supporting Electrolyte:
A good supporting electrolyte has these characteristics:
 It is highly soluble in the solvent chosen.
 It is chemically and electrochemically inert in the
conditions of the experiment.
 Large supporting electrolyte concentrations are
necessary to increase solution conductivity.
 It can be purified.

42. 42
Solvent:
A good solvent has these characteristics:
 It is liquid at experimental temperatures.
 It dissolves the analyte and high concentrations of the
supporting electrolyte completely.
 It is stable toward oxidation and reduction in the
potential range of the experiment.
 It does not lead to deleterious reactions with the
analyte or supporting electrolyte.

43. 43
Factors affecting the electrode reaction
rate:
Mass transfer (e.g., from
bulk solution to the
electrode surface)
Chemical reactions
preceding or
following the electron
transfer.Electron transfer at
the electrode
surface.
Other surface
reactions.

44. 44
Experimental Control:
• Solvent
• Supporting Electrolyte
• Concentrations
Chemical
• Temperature
• Atmosphere
Environmental
• Initial, Switching and Final Potentials
• Scan rate
• Number of sweeps
• Electrodes
Conditions

45. 45

46. 46
 2 mM standard solution of
Potassium Ferricyanide and 1 M
KNO3 solution was prepared using
the 25 mL volumetric flask
provided.
 Magnetic beat used in
the experiment.
 Alu mina pow de r. Polishing Pad.

47. 47
 The working electrode was polished using the alumina slurry
polishing pad and rinsed well with Distilled water and then
dried.

48. 48 Polishing of Working Ele ctrode .
As the electrochemical
event of interest occurs at
the working electrode
surface, it is imperative
that the electrode surface
be extremely clean and its
surface area well-defined.

49. 49
 The working electrode, reference electrode (Ag/AgCl in 1 M KCl)
and counter electrode was placed into the electrochemical cell. It
was ensured that the electrodes are suspended in solution i.e.
that they are not touching the bottom of the cell

50. 50
 The potentiostat cables were connected to the electrodes
accordingly (black: Platinum working electrode, white: Ag/AgCl
reference electrode and red: Platinum wire counter electrode).

51. 51
 Nitrogen Purging with Distilled water before taking the CV.

52. 52
 The nitrogen flow is
started at a rate that
the nitrogen bubbles
slowly through the
solution while the
solution is stirred.
 Once the purge time is
completed, the stirred
and the nitrogen flow are
discontinued.
 Nitrigen purging.

53. 53
 The electrochemical cell was filled
with about 8 to 10 mL of the
Ferricyanide solution and placed in
cell holder.
 N i t r o g e n C y l i n d e r

54. 54
 Setting of the experimental parameters according to
the requirement in the Change Parameters Dialog box.
Once the changes are entered, an experiment using
these parameters can be run by clicking on RUN button
in the dialog box.

55. 55
 Plotting of Cyclic Voltammogram.
 After the experiment has been run, the
voltammogram is displayed.

56. A. Initial negative current.
(No current between A & B (+0.7 to +0.4V) as
no reducible or oxidizable species present in this
potential range)
B. At 0.4V, current begins because of the
following reduction at the cathode:
Fe(CN)6
3- +e- » Fe(CN)6
4-
56
B-D. Rapid increase in current as the surface
concentration of Fe(CN)6
3- decreases.
D. Cathodic peak potential (Epc) and peak current
(ipc).
D-F. Current decays rapidly as the diffusion layer
is extended further from electrode surface.
F. Scan direction switched (-0.15V), potential
still negative enough to cause reduction of
Fe(CN)6
3-
F-J. Eventually reduction of Fe(CN)6
3- no longer
occurs and anodic current results from the
reoxidation of Fe(CN)6
4-
J. Anodic peak potential (Epa) and peak current
(ipa).
K. Anodic current decreases as the accumulated Fe(CN)6
4- is used up at
the anodic reaction.

57. 57
Important Quantitative Information:
 ipc = ipa
 ∆ Ep = (Epa – Epc) = 0.0592MV / n,
where n = number of electrons in reaction
 The formal potential for a reversible couple:
E 0 = midpoint of Epa  Epc
E O = (Ep,a + Ep.c)/2
 ip = (2.686x105)n3/2ACD1/2v1/2
- A: electrode area
- C: concentration
- v: scan rate
- D: diffusion coefficientThus,
- can calculate standard potential for half-reaction
- number of electrons involved in half-reaction
- diffusion coefficients
(if reaction is reversible)

58. 58
Single Electron Transfer Process
Three types of single electron transfer process can be
studied:
 Reversible process
 Irreversible process
 Quasi-reversible process

59. 59
Reversible electron transfer process:
In this process the rate of reaction is fast enough to
maintain equal concentration of the oxidized and reduced
species at the surface of electrode. The concentration
Cox and Cred of oxidized and reduced forms of the redox
couple respectively follow the Nernst equation-
Where, n= no. of electrons transferred,
F= Faraday constant,
R= Gas constant and
T=temperature.
E = E° - RT/nF (ln Cox / Cred)

60. 60
 If the system is diffusion controlled then under that
condition, peak current is given by Randles Sevcik
equation;
where, n is the stoichiometric number of electrons
involved in the electrode reaction,
A is the area of electrode in Cm2
D0 is the diffusion coefficient of the species O in Cm2s-1
C0 is the concentration of the species O in mol/cm-3 and
v is the scan rate in Vs-1.
ip = (2.69 X 105) n3/2 A D1/2 C0 v1/2

61. 61
Diagnostic tests for cyclic voltammograms of
reversible system at 25 °C
∆Ep = Epa-Epc = 59 mV /n,
where n is number of
electrons change
ipc/ipa = 1
ip α v1/2
Ep is independent of v

62. 62
Irreversible electron transfer process:
 For an irreversible process, only forward oxidation or
reduction peak is observed but at times with a weak
reverse peak.
 This process is usually due to slow electron exchange
or slow chemical reactions at the electrode surface
 In an irreversible electrode process, the mass transfer
step is very fast as compared to the charge transfer
step.
 The value of Ep, the difference between the cathodic
and anodic peak is of the order of 59mV/n.
 The peak separation Ep is a factor determining the
reversibility or irreversibility of an electrode reaction.

63. 63
no reverse peak
ipc/ipa = 1
Ip α v1/2
Diagnostic tests for cyclic voltammograms of
irreversible system at 25 °C

64. 64
Quasi-reversible electron transfer process:
This is a class of electrode reactions in which the rates
of charge transfer and mass transfer are comparable or
competitive.
Quasi-reversible process is intermediate between
reversible and irreversible systems.
The current due to quasi-reversible processes is
controlled by both mass transport and charge transfer
kinetics.
The process occurs when the relative rate of electron
transfer with respect to that of mass transport is
insufficient to maintain Nernst equilibrium at the
electrode surface.
In the quasi-reversible region both forward and backward
reactions make a contribution to the observed current.

65. 65
Ip increases with scan rate,
but is not proportional to
scan rate.
∆Ep is greater than 59mV/n
and it increases with
increasing scan rate.
Diagnostic tests for cyclic voltammograms of
Quasi-reversible system at 25 °C

66. 66
Electrochemical Mechanisms Involving
Coupled Chemical Reactions:

67. 67

68. 68
 Study of Reaction Mechanisms-
CV can provide information about the chemistry
of redox couples. One of the most important
applications of cyclic voltammetry is for qualitative
diagnosis of the chemical reaction that precede or
succeed the redox process. Change in the shape of
cyclic voltammogram can be extremely useful for
elucidating the reaction pathways and for providing
reliable chemical information about reactive
intermediates.

69. 69
Quantitative Determination-
Concentration of analyte, Number of electrons per
molecule in analyte and Diffusion coefficient.
Electrochemical Reversibility-
To evaluate electrochemical reversibility by looking at
the difference between the peak potentials for the anodic
and the cathodic scans.
 Study of Characterisation-
Cyclic voltammetry is a very important analytical
characterization in the field of electrochemistry. Any
process that includes electron transfer can be investigated
with this characterization.

70. 70
Corrosion studies in CV:
Cyclic sweeps are used to measure corrosion that
proceeds at about the same rate all over the metals
surface (uniform) and corrosion at discrete sites on the
surface.
Study of adsorption process:
CV can also be useful for evaluating the interfacial
behaviour of electro active compounds.

71.  A wide range of current over potentials.
 Fast technique (single scans typically recorded in every
100 ms).
 Low signal to noise ratio.
 Idea about reversibility of the reaction i.e. The product
of the electron transfer reaction that occurred in the
forward scan can be probed again in the reverse scan.
 Complete electrochemical information obtained.
 Can determine mechanisms and kinetics of redox
reactions.
71

72. 72
 Cyclic voltammetry has become a popular tool in the
last fifteen years for studying electrochemical
reactions.
 Organic chemists have applied the technique to the
study of biosynthetic reaction pathways and to
studies of electrochemically generated free radicals.
 An increasing number of inorganic chemists have been
using cyclic voltammetry to evaluate the effects of
ligands on the oxidation/reduction potential of the
central metal ion in complexes and multinuclear
clusters. This type of information plays an integral
part in many of the approaches directed towards solar
energy conversion and in model studies of enzymatic
catalysis

73. 73
CV is rarely used for quantitative determinations, but it
is widely used for:-
The study of redox processes,
For understanding reaction intermediates, and
For obtaining stability of reaction
And,
Generally used to study the electrochemical properties of
an analyte in solution.

74. 74
D E C EMB ER T O M A R C H
Lite ratu re
Re v ie w
M A R C H - A P R I L
Writing
The sis
A P R I L
Proj e ct
Pre se ntation
And The sis
Su bmission

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Books Referered:
 ELECTROCHEMICAL METHODS - Fundamentals and Applications by
Allen J. Bard & Larry R. Faulkner (second edision).
 ELECTROCHEMISTRY - Principles, Methods, and Applications by
Christopher M. A. Brett and Ana Maria Oliveira Brett
 ELECTROANALYTICAL METHODS - Guide to Experiments and
Applications by A.M. Bond, R.G. Compton, D.A. Fiedler, G. Inzelt, H.
Kahlert, Š. Komorsky-Lovri´c, H. Lohse, M. Lovri´ c, F. Marken, A.
Neudeck, U. Retter, F. Scholz, Z. Stojek.
 CYCLIC VOLTAMMETRY – Simulation and Analysis of Reaction
Mechanisms by David K. Gosser, Jr.

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Firstly, I would like to express my special thanks of gratitude to our
HOD, Dr. A.N. Acharya Sir as well as my Guide, Dr. B.R. Das Sir who
gave me the golden opportunity to do this wonderful review project
on the topic “CYCLIC VOLTAMMETRY”, which also helped me in doing
a lot of research and I got to know about so many things. I am also
thankful to all my teachers for their graceful extended hands.
Secondly, I would like to thank all my friends who helped me a lot.
To great extent it helped me in improving my knowledge and skills.
Lastly, I would like to thank The Almighty for enabling me to
successfully represent this presentation in front of everyone.

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