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Amperometry

This document discusses the working of amperometry and different types of amperometric titration curves. It describes the steps involved in an amperometric titration including introducing the solution, adjusting applied voltage, bubbling with nitrogen gas, recording current and burette readings, and plotting the curve. It classifies amperometric curves into three types depending on whether the titrand, titrant, or both are reducible species. When the titrand is reducible, the current decreases until the endpoint is reached. When the titrant is reducible, no current flows until the endpoint. When both are reducible, the curve is V-shaped as current first decreases then increases again.

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292 views5 pages

Amperometry

This document discusses the working of amperometry and different types of amperometric titration curves. It describes the steps involved in an amperometric titration including introducing the solution, adjusting applied voltage, bubbling with nitrogen gas, recording current and burette readings, and plotting the curve. It classifies amperometric curves into three types depending on whether the titrand, titrant, or both are reducible species. When the titrand is reducible, the current decreases until the endpoint is reached. When the titrant is reducible, no current flows until the endpoint. When both are reducible, the curve is V-shaped as current first decreases then increases again.

Uploaded by

Mr Daniel
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd

Submitted To:

Ma'am Parveen Kanwal

Submitted By:
Anum Iftikhar (MPCHE-22-3)

Subject:
Advance Electroanalytical Techniques (CHE-523)

Topic:
Working of Amperometry

Discipline:
M.Phil. Analytical Chemistry

1st Semester (2022-2024)

1
Working:
a. A known volume of the solution under investigation is introduced in the titration cell,
b. The apparatus is assembled and electrical connections are duly completed with
dropping mercury electrode (C) as cathode and saturated calomel half-cell as anode.
c. A slow stream of pure analytical grade Nitrogen gas is bubbled through the solution
for 15 minutes to get rid of dissolved Oxygen completely.
d. Applied voltage is adjusted to the desired value, and the initial diffusion current (Id)
is noted carefully.
e. A known volume of the reagent is introduced from the semi micro burette (B).
f. Nitrogen is again bubbled through the solution for about 2 minutes to ensure thorough
mixing as well as complete elimination of traces of Oxygen from the added liquid.
g. The flow of Nitrogen gas through the solution is stopped, but is continued to be
passed over the surface of the solution gently so as to maintain an Oxygen free inert
atmosphere in the reaction vessel.
h. The current (µA) and micro burette readings are recorded simultaneously
i. The procedure is repeated until sufficient readings have been obtained to allow the
equivalence point to be determined as the intersection of the two linear portions of the
graph thus achieved.

2
Amperometric Curves:
An amperometric titration curve is a plot of current as a function of titrant volume. The shape
of the curve varies depending on which chemical species (the titrant, the analyte, or the product
of the reaction) is electroactive.

Classification of Amperometric Curves:


Amperometric titration can be divided into types:

A. Titrand is reducible species:


Titration of Lead ions with sulphate or oxalate ions.
Sample is taken in titration cell and soleplate ions are taken in micro-burette.
Lead ions are reduced to Lead. Ultimately, precipitates of Lead Sulphate are formed. As
there is decrease in concentration of ionic form, the diffusion current also decreases. It
becomes minimum at end point. After the end point further addition of titrant does not
produce diffusion current.

B. Titrant as reducible species:


In this case the titration proceeds with no current flow till the equivalence point. As no
species is reduced. However, at the equivalence point the added titrant is reduced and
current is steadily increased.
Example: Titration of non-reducible Magnesium ions with non-reducible 8-hydroxy
quinoline at a potential of -1.6 Volt (versus SCE)

3
C. Both titrant and titrand are reducible species:
The Current first decreases due to removal of the titrand (reactant)due to reaction with
titrant. The current is minimum at the end point. On further addition of the titrant the
current once again increase. When we plot a graph of current versus volume of titrant a V
shaped curve is obtained.

4
REFERENCES;

1. Polarography and amperometric titration pdf page 56


2. Research Article: https://www.brainkart.com/article/Amperometric-Methods--
Instrumentation_30875/
3. YouTube Video: https://youtu.be/1EWiEENa4Gs
4. YouTube Video: https://youtu.be/Go1zgWHw-hs

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