ALGERIAN DEMOCRATIC AND POPULAR REPUBLIC

Ministry of Higher Education and Scientific Research

The university named Ferhat ABBAS Sétif1.

de travai

FACULTE DES SCIENCES

DEPARTEMNT DE CHIMIE
CHIMIE ANALYTIQUE

MODULE : TP Analytique

TP03 : Electrochemical metering volta with potentiostat's

device.

Réalisé par :GHAMOUD RAID

Enseignante : Dr. A-ADDALA

ANNEE UNIVERSITAIR2023/2024
2022/2023
 Sommaire :

-introduction
-but de manipulation
-partie théorique
-partie pratique
-partie expérimentale
-interprétation
-conclusion
-référence
Introduction
Electrochemistry is the study of the relationship between
electricity and chemical reactions. It involves the study of electron
transfer and primarily focuses on redox reactions. Redox
reactions are reactions that involve both reduction and oxidation.
Therefore, electrochemistry pertains to the transfer of electrons in
redox reactions. In the context of electron transfer, the following
assumptions can be made:

The act of reducing is the process of gaining electrons.

Oxidation refers to the loss of electrons.

Electrochemistry involves the study and quantification of the

controlled release of energy in redox systems. Oxidation-reduction
reactions can occur spontaneously and uncontrollably if you mix
your reactants in a beaker. However, if you separate the reactants
and allow a circuit to form, then the reaction can be controlled.
Remember that oxidation-reduction involves the transfer of
electrons in a system, and connecting the reactants through a
circuit allows electrons to flow through the wires.

Voltammetry is an electroanalytical method that is directly related

to the characteristics of electrochemical reactions. It is based on
measuring the current flow resulting from the reduction or
oxidation of compounds present in solution under the controlled
variation of potential difference between two specific electrodes.
The fundamental characteristics of an electrochemical reaction
 can be determined by measuring the current variations with
applied potential in an electrolysis cell. This experimental
determination of the relationship between current and electrode
potential results in obtaining figures called voltammograms. Thus,
the general principle of voltammetry is obtaining a response
(current) from the system being studied to the excitation
(potential) responsible for the desired electrochemical reaction.
This is achieved by exploring and progressively varying the
electrode potential (potential scan). To be able to impose and vary
the electrode potential to produce electrochemical reactions, it is
necessary to operate in an electrolysis cell with three electrodes
connected to an external circuit. The potential of the main
electrode where the desired reactions are to occur, known as the
indicator electrode (or working electrode), can be controlled with
the help of a reference electrode. Electrolysis is manifested by the
flow of electric current, the intensity of which can be measured in
the external circuit using the third electrode known as the counter
electrode.

But de manipulation :
.identifier et de mesurer quantitativement un grand nombre de composés
(cations, certains anions, composés organiques), dont certains
simultanément, et également d’étudier les réactions chimiques incluant
ces composés1.. mesure du flux de courant résultant de la réduction ou
de l’oxydation des composés tests présents en solution sous l’effet d’une
variation contrôlée de la différence de potentiel entre deux électrodes
spécifiques1..Étude la réactivité électrochimique de la masse active de
Fe3+..Détermine le domaine d’électro activité.
 Quantitative Analysis of Cations, Anions, and Organic
Compounds: A Comprehensive Approach
  Exploring Chemical Reactions: How Electrochemical
Measurements Can Shed Light
 Understanding Electrochemical Reactivity: Investigating the Active
Mass of Fe3+
 Unveiling the Hidden Potential: The Role of Potential Difference in
Redox Reactions
 Advancing Electrochemical Studies: Detailed Insights into
Compound Reduction and Oxidation
 Going Beyond the Surface: Mapping the Electroactive Domain for
Comprehensive Analysis
 Harnessing Electrochemistry: A Powerful Tool for Analyzing
Multiple Compounds Simultaneously
 Taking Control of the Current Flow: Analyzing Flux and Its
Relationship to Redox Reactions
 Opening New Doors in Chemical Research: How Electrochemistry
Can Revolutionize Analysis
 From Theory to Practice: Electrochemical Techniques for
Quantitative Compound Testing

Partie théorique :
The fundamental characteristics of an electrochemical reaction
can be determined by measuring the variations in current as a
function of the applied potential in an electrolysis cell. This
experimental determination of the relationship between current
and electrode potential is known as voltammetry. The general
principle of voltammetry involves obtaining a response (current)
from the system being studied to the stimulation (potential)
responsible for the desired electrochemical reaction. This is
achieved by exploring and gradually varying the electrode
potential (potential scanning). To control and vary the electrode
potential in order to induce electrochemical reactions, a three-
electrode electrolysis cell connected to an external circuit is used.
The potential of the electrode where the desired reactions occur,
known as the indicator electrode (or working electrode), can be
controlled with the help of a reference electrode. Electrolysis is
manifested by the flow of electric current, which can be measured
on the external circuit, using the third electrode called the counter
electrode (usually not controlled itself). The electrode through
which the current flows in the direction of reduction is called the
cathode, while the electrode through which the current flows in the
direction of oxidation is called the anode. Reversal of the current
direction in the circuit (during potential variation) reverses the
roles of the two electrodes. To impose and control the potential of
the indicator electrode, an electronic control device called a
potentiostat is used, to which the three electrodes are connected.
This device automatically provides the necessary voltage between
the indicator electrode and the counter electrode to maintain the
voltage between the indicator electrode and the reference
electrode at a set value displayed on the device. To describe a
voltammogram, the potential is gradually varied by modifying the
set voltage controlled by the potentiostat, using an automatic
control system. Automated measurement of the current can also
be performed and recorded as a function of potential, point by
point. Complete automation of the tracing allows for the recording
of the voltammogram. In addition to the essential aspect related to
the experimental procedure for determining voltammograms, it is
important to consider the different types of indicator electrodes.
Here, we will focus on solid indicator electrodes. For a given
reaction, the shape of the voltammetric response depends on a
crucial factor, which is the diffusion transport regime of the
electroactive species in solution. Thus, there are several
voltammetric methods that distinguish themselves by different
instrumental specificities. With an indicator electrode device that
allows operation in a stationary convective diffusion regime
(rotating indicator electrode device), the method is called
stationary voltammetry or hydrodynamic voltammetry. Achieving
stationary diffusion requires relatively slow potential scanning. The
voltammograms obtained in the absence of any convection, i.e., in
a pure natural diffusion regime (immobile indicator electrode
device, as well as the electrolyte solution), have a different
morphology from the former and correspond to another form of
voltammetry. These voltammograms are mainly dependent on the
scanning rate, which can be very high. Moreover, performing a
forward and backward scanning results in voltammograms with
different shapes. The method corresponding to this procedure is
called cyclic voltammetry. Both hydrodynamic voltammetry and
cyclic voltammetry are electroanalytical methods based on
measurements under dynamic microelectrolysis conditions (non-
equilibrium conditions). The obtained curves (which are
characteristic of the electrolyte solution) can be used for analytical
purposes to determine the nature and concentration of present
reducible or oxidizable species. Knowledge of the evolution of the
voltammograms during a reaction allows for monitoring its
progress and thus developing, for example, amperometric or
potentiometric detection methods. Voltammetric curves can also
be used to measure kinetic parameters, either electrochemical
kinetics or chemical kinetics when a chemical reaction is coupled
with an electrochemical reaction. Similarly, the conditions under
which coulometry or coulometric titration should be carried out can
be determined using the voltammogram trace.

Gaining knowledge about the fundamental principles of

electrochemical reactions by studying voltammetry

Exploring the Relationship between Current and Electrode Potential with

Voltamperograms
The Role of Potentiostats in Controlling Electrode Potentials for
Voltammetry
Different Types of Electrodes for Voltammetric Analysis
Unveiling the Secrets of Voltammetry: Hydrodynamic vs. Stationary
Analysis
Analyzing Electrolytic Solutions with Dynamic Microelectrolysis
Techniques
Using Voltamperograms to Determine the Nature and Concentration of
Redox Species
Ampere vs. Potential Detection: Choosing the Right Method for Analysis
Examining Kinetics with Voltammetry: Electrochemical and Chemical
Reactions
Coulometry and Coulometric Analysis: Determining Conditions with
Voltamperograms
A potentiostat is an electronic instrument designed to control the
potential of the working electrode in a multi-electrode
electrochemical cell. It contains various internal circuits that allow
it to function in this manner. The circuits generate and measure
potentials and currents. In a conventional three-electrode cell, the
cell cable is connected to the working, auxiliary (or counter), and
reference electrodes at one end, and to the potentiostat's cell
cable connector at the other end. The potentiostat's internal circuit
controls the applied signal. In the case of potential-controlled
methods, for example, the potential of the working electrode is
maintained relative to the reference electrode. At the same time,
current flows between the working and auxiliary electrodes. The
design of the potentiostat circuit prevents anything but a
minuscule current from flowing between the working and
reference electrodes at high impedance.

What You Should Be Aware of About Potentiostats

Gaining comprehension of the internal circuits within a

potentiostat.
The method by which a potentiostat manages and assesses
electrical potentials and currents.

Investigating the Use of Three Electrodes in Electrochemical Cells

The internal circuit of the potentiostat plays a crucial part in

controlling the signal.

Keeping the effectiveness of functioning electrodes intact through

the usage of potentiostats.

Explanations of the Flow of Electric Current Between Functional

and Supplemental Electrodes

Impedance in Potentiostats: Avoiding Undesired Currents

Benefits and Uses of Potential Methods Controlled by Potentiostat

Uncover the Capabilities of Potentiostat Circuit Design.

1
.
 The advantages of utilizing a bipotentiostat and
polypotentiostat in electrochemical experiments.

 The enhancement of experimental efficiency and accuracy

can be achieved through the utilization of modern
potentiostats.
 Investigating the flexibility of potentiostats equipped with
numerous functioning electrodes.

 Improving the analysis of data in the field of electrochemistry

by utilizing potentiostats connected to computers.

 Grasping the Distinction Between Voltammetry and

Voltametry in Electrochemical Measurements

 Unleashing the Potential of Potentiostats: A Summary of

How They Work

 Making electrochemical research more efficient through the

use of automated software for potentiostats.

 The development of potentiostats: From independent devices

to computer-managed solutions.

 Expanding the Boundaries of Electrochemistry with

Advanced Potentiostats
 Increasing the versatility of experiments by utilizing
polypotentiostats with multiple channels
Partie logiciel
LES MATRIALE ET LES PRODUIT
LES MATRIALE LES PROUDUIT
L’EAU DISTILLE
LOGICIEL DE VOLTAMASTER 4
KCl
L’APPARAIL POTONTIOSTAT
K3FeCN6
BECHER
LES ELECTRODE
( AUXILIARE .TRAVAIL.REFERENCE )
ORDINATEUR
PALANCE ANAYTIQUE
SPATUL
VERR DE MONTRE

Partie expérimentale
LES CALCULE
On chercher la masse de Fe2+ ; n=c*v m/M=c*v et
m=c*v*M
LA MASSE MOLAIRE DE k2FeCN6=329.24g/mol v=50ml
C0=2*10^-3 donc m0=0.032g
Donne la concentration connu
C1=4*10-3 M et la masse m1=50*10 ^-3*329.24*4*10^-
3=0.065g {potentiel=131,5mV et Courant= -26,31µA}
C2=6*10-3 M et m2= 0.0987g {potentiel=131,5mV et Courant= -
40,99µA}
C3=8*10-3 M et m3=0.131g {potentiel=131,5mV et Courant= -
55,15µA}
C4=10*10-3 M et m4=0.164g {potentiel=131,5mV et Courant= -
67,78µA}
C(inconnue) {potentiel=131,5mV et Courant= -54,51µA
Partie pratique
 Investigating the responsiveness of Fe3+ ions
through the utilization of a potentiostat and
electrodes.

 The current density and potential of KCl are being analyzed

using Volume Master 4 Software.

 Examining the actions of Fe3+ ions using the technique of

mass addition

 Gaining knowledge about the correlation between mass and

potential in electrochemical analysis

 Investigating the reactivity of Fe3+ ions by adding multiple

masses.

 Revealing the Impact of KCl on the Density of Current and

Potential

 The Dilution Technique is used in Electrochemical Analysis

to determine the concentration of an unknown substance (C).
 Examining the concentrations of electric charge and possible
electric charge in the existence of water, potassium chloride,
and iron (III) ions.

 Using a Potentiostat and electrodes to analyze the reactivity

of ions.

 Conducting research in the field of electrochemistry to

examine the correlation between mass, concentration, and
potential.
Conclusion :
A potentiostat is a gadget that adjusts the voltage of the working
electrode in a complex electrochemical cell with many electrodes. It
helps to explore electrochemical events, such as redox reactions. Modern
potentiostats are shrinking and becoming more handy, making them
more suitable for use beyond the lab.
Voltammetry is a technique that measures the current that emerges from
the oxidation or reduction of substances in a solution under the impact of
a controlled change of the voltage gap between two specific electrodes. It
enables the discovery and estimation of many substances, as well as the
study of chemical reactions involving these substances.
To wrap up, the potentiostat and voltammetry are useful tools in
electrochemistry. The potentiostat is used to fine-tune electrode voltage
and measure current, while voltammetry is used to scrutinize
electrochemical reactions by measuring current as a function of applied
voltage. These two tools are crucial for the analysis and comprehension
of electrochemical events.
Référence :
https://chimieanalytique.com/potentiometrie/
https://fr.wikipedia.org/wiki/%C3%89lectrochimie
https://www.techniques-ingenieur.fr/base-documentaire/archives-
th12/archives-techniques-d-analyse-tiata/archive-2/voltamperometrie-
sur-electrode-solide-introduction-p2125/
https://pineresearch.com/shop/kb/theory/instrumentation/what-
potentiostat-does/
https://fr.wikipedia.org/wiki/Voltamp%C3%A9rom%C3%A9trie
https://fr.wikipedia.org/wiki/Potentiostat
https://fr.wikipedia.org/wiki/Voltamp%C3%A9rom%C3%A9trie