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Description of Electrochemical

Techniques

The technique is named according to the

parameters measured

E.g.

Voltammetry measure current and

voltage

Potentiometry measure voltage

Chrono-potentiometry measure voltage

with time (under an applied current)

Chrono-amperometry measure current

with time (under an applied voltage)

Electro-Kinetics

Movement of Ions

Butler Volmer Equation

Rotating Disc Electrode

Rotating Cylinder Electrode

Voltammetry

Cyclic Voltammetry

Chrono-potentiometry

Chrono-amperometry

Diffusion Movement under a concentration

gradient. If an electrochemical reaction occurs the

current due to this reaction is called, id , the

diffusion current.

Migration or Transport Movement of ions under

an electric field due to coulombic forces. If an

electrochemical reaction occurs the current due to

this reaction is called, im , the migration current.

Convection Movement due to changes in density

at the electrode solution interface. This occurs due

to depletion or addition of a species due to the

electrochemical reaction.

The charging or capacitance current, ic , is due to

the presence of the electrical double layer and it

is always present. This current, of course, is not

related to any movement of ions.

Ic = Cdl x V

Where:

Cdl = the capacitance of the electrical double

layer

V = voltage scan rate

The capacitance current makes its presence felt

when measuring charge transfer (Faradaic)

processes at concentrations of 10 -5 M.

Diffusion

Molecular

diffusion, often

called simply

diffusion, is a net

transport of

molecules from a

region of higher

concentration to

one of lower

concentration by

random molecular

motion.

Migration or Transport

Is the fraction of current carried by the ions.

For example in a solution of copper sulphate the

transport number of Cu2+ is 0.4 and that of SO42- = 0.6.

t+ + t- = 0.4 + 0.6 = 1

Since the migration current depends on the ionic

strength of the solution it is usually eliminated by

addition of excess of an inert supporting electrolyte (100

1000 fold excess in concentration)

The current is carried by the inert supporting electrolyte

(e.g. NaCl , KNO3 etc) because the ions produced do

not undergo any electrochemical reaction the transport

current is effectively removed.

In excess inert supporting electrolyte, the current

measured due to the electro-active species of interest is

due only to diffusion which can be related to mass

transfer.

the migration current is eliminated. Pb2+ + 2e Pb0

The supporting electrolyte

Ensures diffusion control of limiting currents by

eliminating migration currents

Table: Limiting currents observed for 9.5 x 10-4 M

PbCl2 as a function of the concentration of KNO3

supporting electrolyte

Molarity

of KNO3

0

Il

A

17.6

0.001

12.0

0.005

9.8

0.10

8.45

1.0

8.45

Voltammetry

The example shown is for the reduction of Pb2+

at an inert mercury electrode.

Pb2+ + 2e Pb(Hg)

At low inert electrolyte concentration a large

fraction of the total current is due to the

migration current, i.e. the currents due to the

electrostatic attraction of ions to the electrode.

For solution 1:

i migration im 17.6 8.45 = 9.2 A

i diffusion

id = 8.45 A

Fick's first law relates the diffusive flux

to the concentration field, by postulating

that the flux goes from regions of high

concentration to regions of low

concentration, with a magnitude that is

proportional to the concentration gradient

(spatial derivative).

In one (spatial)

J this

Dis

dimension,

J D

x

where

J is the diffusion flux in dimensions of [(concentration

of substance) length2 time-1], example mole (M) m-2 s1.

J measures the amount of substance that will flow

through a small area during a small time interval.

D is the diffusion coefficient or diffusivity in

dimensions of [length2 time1], example m2 s-1

(for ideal mixtures) is the concentration in

dimensions of [(concentration of substance) length 3],

example M m-3

x is the position [length], example m

D is proportional to the squared velocity of

the diffusing particles, which depends on

the temperature, viscosity of the fluid and

the size of the particles according to the

Stokes-Einstein relationship.

In dilute aqueous solutions the diffusion

coefficients of most ions are similar and

have values that at room temperature are

in the range of 0.6x10-9 to 2x10-9 m2/s.

For biological molecules the diffusion

coefficients normally range from 10-11 to

10-10 m2/s.

In two or more dimensions we must use, ,

the del or gradient operator, which

generalises the first derivative, obtaining

J = -D

The driving force for the one-dimensional

diffusion is the quantity -/x

which for ideal mixtures is the concentration

gradient. In chemical systems other than ideal

solutions or mixtures, the driving force for

diffusion of each species is the gradient of

chemical potentialDc

of this

species. Then Fick's

J i 1 i case) can be

RT x

written as:

Dc1 i

Ji

RT x

c is the concentration (mol/m3),

R is the universal gas constant (J/(K mol)),

T is the absolute temperature (K), and

is the chemical potential (J/mol).

Butler-Volmer Equation

The Butler-Volmer equation is one

of the most fundamental

relationships in electrochemistry. It

describes how the electrical current

on an electrode depends on the

electrode potential, considering that

both a cathodic and an anodic

reaction occur on the same

electrode:

Butler-Volmer Equation

where:

I = electrode current, Amps

Io= exchange current density, Amp/m2

E = electrode potential, V

Eeq= equilibrium potential, V

A = electrode active surface area, m2

T = absolute temperature, K

n = number of electrons involved in the electrode reaction

F = Faraday constant

R = universal gas constant

= so-called symmetry factor or charge transfer

coefficient dimensionless

The equation is named after chemists John Alfred Valentine

Butler and Max Volmer

Butler-Volmer Equation

The equation describes two regions:

At high overpotential the Butler-Volmer

equation simplifies to the Tafel equation

E Eeq = a blog(ic) for a cathodic reaction

E Eeq = a + blog(ia) for an anodic reaction

Where:

a and b are constants (for a given reaction and

temperature) and are called the Tafel equation

constants

At low overpotential the Stern Geary equation

applies

Reactions

Without concentration

and therefore mass

transport effects to

complicate the

electrolysis it is

possible to establish

the effects of voltage

on the current

flowing. In this

situation the quantity

E - Ee reflects the

activation energy

required to force

current i to flow.

Plotted below are

three curves for

differing values of io

with = 0.5.

Voltammetry

Although the Butler Volmer Equation predicts,

that at high overpotential, the current will

increase exponentially with applied voltage, this

is often not the case as the current will be

influenced by mass transfer control of the

reactive species.

Take the following example of the reduction of

ferric ions at a platinum rotating disc electrode

(RDE).

Fe3+ + e = Fe2+

The rotation of the electrode establishes a well

defined diffusion layer (Nernst diffusion layer)

The contribution of the capacitance current will

also be demonstrated in this example.

Ferric Chloride is carried out in the presence of 1 M NaCl to

eliminate the migration current.

(a)

ild

Slope due to ic

Current

10 M Fe

-3

3+

Fe

3+

+ e Fe

(b)

2+

ild

Current

is recorded at a much higher

sensitivity than in Fig. (b).

Charging Current or

Capacitance Current

Note that due to the presence of the

electrical double layer a charging or

capacitance current is always

present in voltammetric

measurements.

Butler-Volmer Equation

where:

I = electrode current, Amps

Io= exchange current density, Amp/m2

E = electrode potential, V

Eeq= equilibrium potential, V

A = electrode active surface area, m2

T = absolute temperature, K

n = number of electrons involved in the electrode reaction

F = Faraday constant

R = universal gas constant

= so-called symmetry factor or charge transfer

coefficient dimensionless

The equation is named after chemists John Alfred Valentine

Butler and Max Volmer

While the Butler-Volmer equation is valid over the full

potential range, simpler approximate solutions can be

obtained over more restricted ranges of potential. As

overpotentials, either positive or negative, become larger

than about 0.05 V, the second or the first term of

equation becomes negligible, respectively. Hence, simple

exponential relationships between current (i.e., rate) and

overpotential are obtained, or the overpotential can be

considered as logarithmically dependent on the current

density. This theoretical result is in agreement with the

experimental findings of the German physical chemist

Julius Tafel (1905), and the usual plots of overpotential

versus log current density are known as Tafel lines.

The slope of a Tafel plot reveals the value of the transfer

coefficient; for the given direction of the electrode

reaction.

Butler-Volmer Equation

1 nF a

ia ` i0 exp

RT

nF c

ic ` i0 exp

RT

ia and ic are

the exhange

current

densities for

the anodic

and cathodic

reactions

the Tafel equation which was obtained

experimentally

c

RT

RT

ln i0

ln ic

c nF

c nF

0.059

0.059

log i0

log ic at 250 C for the cathodic process

cn

cn

0.059

0.059

a

log i0

log ia at 250 C for the anodic process

an

an

The equation is the well known Tafel equation

a b log i

and

0.059

a

ln io

n

0.059

b

n

Tafel Equation

The Tafel slope is an intensive parameter and does

not depend on the electrode surface area.

i0 is and extensive parameter and is influenced by

the electrode surface area and the kinetics or speed

of the reaction.

Notice that the Tafel slope is restricted to the

number of electrons, n, involved in the charge

transfer controlled reaction and the so called

symmetry factor, .

n is often = 1 and although the symmetry factor can

vary between 0 and 1 it is normally close to 0.5.

This means that the Tafel slope should be close to

120 mV if n = 1 and 60 mV if n = 2.

Tafel Equation

We can write:

RT

ln i i0 or b ln i i0

nF

where

2.303RT

b

the Tafel slope

nF

ln i 2.303 log i

Reactions

Without concentration

and therefore mass

transport effects to

complicate the

electrolysis it is

possible to establish

the effects of voltage

on the current

flowing. In this

situation the quantity

E - Ee reflects the

activation energy

required to force

current i to flow.

Plotted below are

three curves for

differing values of io

with = 0.5.

Tafel Equation

The Tafel equation can be also written as:

where

the plus sign under the exponent refers to an

anodic reaction, and a minus sign to a cathodic

reaction, n is the number of electrons involved in

the electrode reaction k is the rate constant for the

electrode reaction, R is the universal gas constant,

F is the Faraday constant. k is Boltzmann's

constant, T is the absolute temperature, e is the

electron charge, and is the so called "charge

transfer coefficient", the value of which must be

between 0 and 1.

Tafel Equation

The following equation was obtained

experimentally

a b log i

Where:

= the over-potential

i = the current density

a and b = Tafel constants

Tafel Equation

Applicability

Where an electrochemical reaction occurs in two half

reactions on separate electrodes, the Tafel equation is

applied to each electrode separately.

The Tafel equation assumes that the reverse reaction

rate is negligible compared to the forward reaction

rate.

The Tafel equation is applicable to the region where

the values of polarization are high. At low values of

polarization, the dependence of current on polarization

is usually linear (not logarithmic):

due to its formal similarity to Ohms law

Applicable in the linear region of the Butler

Volmer Equation at low over-potentials

icorr

Rp

Where

B the Tafel constant

a c

2.3 a c

R p the measured polarisation resistance

E i

Tafel Equation

Overview of the terms

The exchange current is the current at

equilibrium, i.e. the rate at which oxidized

and reduced species transfer electrons

with the electrode. In other words, the

exchange current density is the rate of

reaction at the reversible potential (when

the overpotential is zero by definition). At

the reversible potential, the reaction is in

equilibrium meaning that the forward and

reverse reactions progress at the same

rates. This rate is the exchange current

density.

Tafel Equation

The Tafel slope is measured experimentally;

however, it can be shown theoretically when

the dominant reaction mechanism involves

the transfer of a single electron that

2.303RT

b

F

T is the absolute temperature,

R is the gas constant

is the so called "charge transfer

coefficient", the value of which must be

between 0 and 1.

Levich Equation

The Levich Equation models the diffusion and

solution flow conditions around a rotating disc

electrode (RDE). It is named after Veniamin

Grigorievich Levich who first developed an RDE as

a tool for electrochemical research. It can be used

to predict the current observed at an RDE, in

particular, the Levich equation gives the height of

the sigmoidal wave observed in rotating disk

voltammetry. The sigmoidal wave height is often

called the Levich current.

In work at a RDE the electrode is usually rotated

quite fast (1000 rpm) in order to establish a well

defined diffusion layer.

The scan rate is relatively slow typically 2-5 mV s 1

It is important to remember that in order to determine the

diffusion current and the mass transfer coefficient using

volatmmetry, excess inert supporting electrolyte must be

present to eliminate the migration current

Levich Equation

The Levich Equation is written as:

where

iL is the Levich current

n is the number of electrons transferred in the half

reaction

F is the Faraday constant

A is the electrode area

D is the diffusion coefficient (see Fick's law of diffusion)

w is the angular rotation rate of the electrode

v is the kinematic viscosity

C is the analyte concentration

While the Levich equation suffices for many purposes,

improved forms based on derivations utilising more

terms in the velocity expression are available. [1][2]

Levich Equation

Levich Equation

Levich Equation

It is important to note that the layer of solution

immediately adjacent to the surface of the

electrode behaves as if it were stuck to the

electrode. While the bulk of the solution is being

stirred vigorously by the rotating electrode, this

thin layer of solution manages to cling to the

surface of the electrode and appears (from the

perspective of the rotating electrode) to be

motionless.

This layer is called the stagnant layer in order to

distinguish it from the remaining bulk of the

solution. The act of rotation drags material to the

electrode surface where it can react. Providing the

rotation speed is kept within the limits that laminar

flow is maintained then the mass transport

The Levich equation takes into account both the

rate of diffusion across the stagnant layer and the

complex solution flow pattern. In particular, the

Levich equation gives the height of the sigmoidal

wave observed in rotated disk voltammetry. The

sigmoid wave height is often called the Levich

current, iL, and it is directly proportional to the

analyte concentration, C. The Levich equation is

written as:

iL = (0.620) n F A D2/3 w1/2 v1/6 C

where w is the angular rotation rate of the

electrode (radians/sec) and v is the kinematic

viscosity of the solution (cm2/sec). The kinematic

viscosity is the ratio of the solution's viscosity to

velocity)

The linear relationship between Levich current and the square

root of the rotation rate is obvious from the Levich plot. A

linear least squares fit of the data produces an equation for

the best straight line passing through the data. The specific

experiment shown, the electrode area, A, was 0.1963 cm 2, the

analyte concentration, C, was 2.55x106 mol/cm3, and the

solution had a kinematic viscosity, v, equal to 0.00916

cm2/sec. After careful substitution and unit analysis, you can

solve for the diffusion coefficient, D, and obtain a value equal

to 4.75x106 cm2/s. This result is a little low, probably due to

the poor shape of the sigmoidal signal observed in this

particular experiment.

The kinematic viscosity is the ratio of the absolute viscosity of

a solution to its density. Absolute viscosity is measured in

poises (1 poise = gram cm1 sec1). Kinematic viscosity is

measured in stokes (1 stoke = cm 2 sec1). Extensive tables of

solution viscosity and more information about viscosity units

can be found in the CRC Handbook of Chemistry and Physics.

Cyclic Voltammetry

Cyclic Voltammetry is carried out at a

stationary electrode.

This normally involves the use of an inert

disc electrode made from platinum, gold or

glassy carbon. Nickel has also been used.

The potential is continuously changed as a

linear function of time. The rate of change

of potential with time is referred to as the

scan rate (v). Compared to a RDE the scan

rates in cyclic voltammetry are usually

much higher, typically 50 mV s-1

Cyclic Voltammetry

Cyclic voltammetry, in which the direction

of the potential is reversed at the end of the

first scan. Thus, the waveform is usually of

the form of an isosceles triangle.

The advantage using a stationary electrode is

that the product of the electron transfer

reaction that occurred in the forward scan can

be probed again in the reverse scan.

CV is a powerful tool for the determination of

formal redox potentials, detection of chemical

reactions that precede or follow the

electrochemical reaction and evaluation of

electron transfer kinetics.

Cyclic Voltammetry

Cyclic Voltammetry

For a reversible

process

Epc Epa = 0.059V/n

Reversible systems

Reversible systems

12

i p 0.4463nFAC nFvD RT

i p 2.687 10 n v D AC

5

32 12

12

v = the scan rate in V s-1

F = the Faradays constant 96,485 coulombs

mole-1

A = the electrode area cm2

R = the gas constant 8.314 J mole -1 K-1

T = the temperature K

D = the analyte diffusion coefficient cm 2 s-1

Reversible systems

As expected a plot of peak height vs the square root of the scan rate

produces a linear plot, in which the diffusion coefficient can be obtained

from the slope of the plot.

Cyclic Voltammetry

Cyclic Voltammetry

Cyclic Voltammetry

Electrode

redox process

E0 = (Epa + Epc ) /2

Separation of peaks for a reversible couple is

0.059/n volts

A one electron fast electron transfer reaction

thus gives 59mV separation

Peak potentials are then independent of scan

rate

Half-peak potential Ep/2 = E1/2 0.028/n

Sign is + for a reduction

Electrode

The shape of the voltammogram depends on the

transfer coefficient

When deviates from 0.5 the voltammograms

become asymmetric -cathodic peak sharper as

expected from Butler Volmer eqn.

Web Sites

http://calctool.org/CALC/chem/electro

chem/levich

http://www.calctool.org/CALC/chem/el

ectrochem/cv1

Tafel Equation

The Tafel slope is an intensive parameter and does

not depend on the electrode surface area.

i0 is and extensive parameter and is influenced by

the electrode surface area and the kinetics or speed

of the reaction.

Notice that the Tafel slope is restricted to the

number of electrons, n, involved in the charge

transfer controlled reaction and the so called

symmetry factor, .

n is often = 1 and although the symmetry factor can

vary between 0 and 1 it is normally close to 0.5.

This means that the Tafel slope should be close to

120 mV if n = 1 and 60 mV if n = 2.

Tafel Equation

We can write:

RT

ln i i0 or b ln i i0

nF

where

2.303RT

b

the Tafel slope

nF

ln i 2.303 log i

Evans Diagrams

Evans Diagrams

Evans Diagrams

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