Polarography is a type of voltammetry where a dropping mercury electrode is used as the working electrode. A polarography cell contains an electrolyte solution, a reference electrode like calomel, a dropping mercury electrode, and an auxiliary electrode. As a potential is applied, the current is measured as mercury droplets fall through the solution. This allows for the analysis of electroactive substances and the production of polarograms that can be used for qualitative and quantitative analysis based on diffusion currents.
The Detailed Theory and instrumentation of Both Amperometry and Biamperometric analysis is given with Titration curves and Applications.
Medha Thakur (M.Sc Chemistry)
The Detailed Theory and instrumentation of Both Amperometry and Biamperometric analysis is given with Titration curves and Applications.
Medha Thakur (M.Sc Chemistry)
It contains what is amperometry and where it will be derived and what is the principle behind the amperometry. Instrumentation of amperometry and the purpose of dipping mercury electrode and rotating platinum electrode. The advantage over rotating platinum electrodes. Amperometric titration curves for reducible ions and non-reducible ions. What tells the Ilkovic equation and how it relates to the amperometry is also included. Applications, advantages, and disadvantages of amperometric titration are also included. Questions related to amperometry and amperometric titration are given for practice. The contents taken from the websites are also given.
The earliest voltammetric technique
Heyrovsky invented the original polarographic method in 1922, conventional direct current polarography (DCP).
It employs a dropping mercury electrode (DME) to continuously renew the electrode surface.
Diffusion is the mechanism of mass transport.
When an external potential is applied to a cell
containing a reducing substance such as CdCl2,
The following reaction will occur:
Cd2+ + 2e + Hg = Cd(Hg)
The technique depends on increasing the applied
voltage at a steady rate and simultaneously
record photographically the current-voltage
curve (polarogram)
The apparatus used is called a polarograph .
When an external potential is applied to a cell
containing a reducing substance such as CdCl2,
The following reaction will occur:
Cd2+ + 2e + Hg = Cd(Hg)
The technique depends on increasing the applied
voltage at a steady rate and simultaneously
record photographically the current-voltage
curve (polarogram)
The apparatus used is called a polarograph .
Capillary tube about 10-15cm
Int. diameter of 0.05mm
A vertical distance being maintained betwwen DME and the solution
Drop time of 1-5 seconds
Drop diameter 0.5mm
The supporting electrolyte
is a solution of (KNO3, NaCl, Na3PO4) in which the sample (which must be electroactive) is dissolved.
Function of the supporting electrolyte
It raises the conductivity of the solution.
It carries the bulk of the current so prevent the
migration of electroactive materials to working
electrode.
It may control pH
It may associate with the electroactive solute as
in the complexing of the metal ions by ligands.
This Power point presentation was prepared to describe in detail about the two main voltammetry techniques of electrochemistry which is polarography and voltammetry. In these slides, I discussed the working, instrumentation, various electrodes, advantages, disadvantages..etc. Hope you understand the topic.
ESTIMATION OF THE RATE OF REACTION WILL BE DONE BASED ON THE POTENTIAL DIFFERENCE BETWEEN REFERENCE AND INDICATOR ELECTRODE. THE POTENTIAL OF THE REFERENCE ELECTRODE IS STABLE WHERE AS THE POTENTIAL OF THE INDICATOR ELECTRODE VARIES WITH THE POTENTIAL OF THE SOLUTION IN WHICH IT IS PLACED
Polarography is a technique used for the qualitative and quantitative analysis of electro reducible or oxidized elements or groups. It is a electrochemical technique of analyzing solution that measure the current flowing between two electrodes in the solution as well as the gradually increasing applied voltage to determine respectively the concentration of solute and its nature.
It contains what is amperometry and where it will be derived and what is the principle behind the amperometry. Instrumentation of amperometry and the purpose of dipping mercury electrode and rotating platinum electrode. The advantage over rotating platinum electrodes. Amperometric titration curves for reducible ions and non-reducible ions. What tells the Ilkovic equation and how it relates to the amperometry is also included. Applications, advantages, and disadvantages of amperometric titration are also included. Questions related to amperometry and amperometric titration are given for practice. The contents taken from the websites are also given.
The earliest voltammetric technique
Heyrovsky invented the original polarographic method in 1922, conventional direct current polarography (DCP).
It employs a dropping mercury electrode (DME) to continuously renew the electrode surface.
Diffusion is the mechanism of mass transport.
When an external potential is applied to a cell
containing a reducing substance such as CdCl2,
The following reaction will occur:
Cd2+ + 2e + Hg = Cd(Hg)
The technique depends on increasing the applied
voltage at a steady rate and simultaneously
record photographically the current-voltage
curve (polarogram)
The apparatus used is called a polarograph .
When an external potential is applied to a cell
containing a reducing substance such as CdCl2,
The following reaction will occur:
Cd2+ + 2e + Hg = Cd(Hg)
The technique depends on increasing the applied
voltage at a steady rate and simultaneously
record photographically the current-voltage
curve (polarogram)
The apparatus used is called a polarograph .
Capillary tube about 10-15cm
Int. diameter of 0.05mm
A vertical distance being maintained betwwen DME and the solution
Drop time of 1-5 seconds
Drop diameter 0.5mm
The supporting electrolyte
is a solution of (KNO3, NaCl, Na3PO4) in which the sample (which must be electroactive) is dissolved.
Function of the supporting electrolyte
It raises the conductivity of the solution.
It carries the bulk of the current so prevent the
migration of electroactive materials to working
electrode.
It may control pH
It may associate with the electroactive solute as
in the complexing of the metal ions by ligands.
This Power point presentation was prepared to describe in detail about the two main voltammetry techniques of electrochemistry which is polarography and voltammetry. In these slides, I discussed the working, instrumentation, various electrodes, advantages, disadvantages..etc. Hope you understand the topic.
ESTIMATION OF THE RATE OF REACTION WILL BE DONE BASED ON THE POTENTIAL DIFFERENCE BETWEEN REFERENCE AND INDICATOR ELECTRODE. THE POTENTIAL OF THE REFERENCE ELECTRODE IS STABLE WHERE AS THE POTENTIAL OF THE INDICATOR ELECTRODE VARIES WITH THE POTENTIAL OF THE SOLUTION IN WHICH IT IS PLACED
Polarography is a technique used for the qualitative and quantitative analysis of electro reducible or oxidized elements or groups. It is a electrochemical technique of analyzing solution that measure the current flowing between two electrodes in the solution as well as the gradually increasing applied voltage to determine respectively the concentration of solute and its nature.
content- Principle
Ilkovic equation
Construction and working of dropping mercury electrode and rotating platinum electrode
Applications
Polarography is a voltammetric technique in which chemical species (ions or molecules) undergo oxidation (lose electrons) or reduction (gain electrons) at the surface of a dropping mercury electrode (DME) at an applied potential. Polarography only applies to the DME.
Objective of polarography
Polarography is an electroanalytical technique that measures the current flowing between two electrodes in the solution (in the presence of gradually increasing applied voltage) to determine the concentration of solute and its nature respectively
Polarography is based upon the principle that gradually increasing voltage is applied between two electrodes, one of which is polarisable (dropping mercury electrode) and other is non-polarisable and current flowing between the two electrodes is recorded.
A sigmoid shape current-voltage curve is obtained from which half wave potential as well as diffusion current is calculated.
Diffusion current is used for determination of concentration of substance.
Half wave potential is characteristic of every element.
Ilkovic equation is a relation used in polarography relating the diffusion current (id) and the concentration of the non-polarisable electrode, i.e., the substance reduced or oxidised at the dropping mercury electrode (polarisable electrode).
Definitions of types of currents
1. Residual current (ir), 2. Migration current (im): , 3. Diffusion current (id) 4.Half wave potential 5. Limiting current (il)
Dropping mercury electrode- Dropping mercury electrode (DME) is a polarisable electrode and can act as both anode and cathode.
The pool of mercury acts as counter electrode,
i.e., anode if DME is cathode or
cathode if DME is anode.
The counter electrode is a non-polarisable electrode.
To the analyte solution, electrolyte like KCl is added i.e., 50-100 times of sample concentration.
Pure nitrogen or hydrogen gas is bubbled through the solution, to expel (remove) out oxygen.
Eg: If the analyte solution contains cadmium ions, then cadmium ions are discharged at cathode (-)
Cd2+ + 2e- → Cd
Then, gradually increasing voltage is applied to the polarographic cell and current is recorded.
Graph is plotted between voltage applied and current. This graph is called Polarograph and the apparatus is known as Polarogram.
The diffusion current produced is directly proportional to concentration of analyte and this is used in quantitative analysis.
The half wave potential is characteristic of every compound and this is used in qualitative analysis.
Graph is plotted between voltage applied and current. This graph is called Polarograph and the apparatus is known as Polarogram.
The diffusion current produced is directly proportional to concentration of analyte and this is used in quantitative analysis.
The half wave potential is characteristic of every compound
Microelectronic technology
This report briefly discusses the need for Metal-Oxide-Semiconductor Field Effect Transistors (MOSFETs), their structure and principle of operation. Then it details the fabrication and characterization of the MOSFETs fabricated at the microelectronic lab at University of Malaya
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Polarographic technique is applied for the qualitative or quantitative analysis of electroreducible or oxidisable elements or groups.
It is an electromechanical technique of analyzing solutions that measures the current flowing between two electrodes in the solution as well as the gradually increasing applied voltage to determine respectively the concentration of a solute and its nature.
The principle in polarography is that a gradually increasing negative potential (voltage) is applied between a polarisable and non-polarisable electrode and the corresponding current is recorded.
Polarisable electrode: Dropping Mercury electrode
Non-polarisable electrode: Saturated Calomel electrode
From the current-voltage curve (Sigmoid shape), qualitative and quantitative analysis can be performed. This technique is called as polarography, the instrument used is called as polarograph and the current-voltage curve recorded is called as polarogram
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Slides from:
11th International Conference on Electrical, Electronics and Computer Engineering (IcETRAN), Niš, 3-6 June 2024
Track: Artificial Intelligence
https://www.etran.rs/2024/en/home-english/
2. Polarography is a subclass of
voltammetry where the working
electrode is a dropping mercury
electrode (DME).
It is current versus potential are recorded
when gradual changing current is take
place when current applied to cell.
3. A cell containing :
Solution of interest (electroactive
substance)
Stable reference electrode. e.g : calomel
electrode.
Small area of indicator electrode (DME)
Auxiliary or counter electrode .
5. Hg will dropped in stable flow rate 5- 30
drops/min.
Volts applied 50 – 200 mv/min
Drop life 2 – 12 sec.
Potential range (+ 0.4) – (-2) V
6. Advantage of Hg electrode
As the Hg capillary very narrow so, able to
analyse very small volume of analyte.
Surface of electrode is very reproducible .
Surface area of electrode can be calculated
from the weight of drops.
10. Factors affecting diffusion
current
(Ilkovic equation)
ίd = 708 n C D½ m ⅔ t⅙
n : change in valency
C : concentration
D : diffusion coefficient.
m: flow rate of mercury dropping.
t : life time of mercury drop.
