06-04-2022
Volumetric Analysis
The method in which the concentration of a substance in a solution is estimated by
adding the same number of compounds of another substance present in a solution of
known concentration is called volumetric analysis. Volumetric Analysis is also known as
Titration.
The titrant is the component whose solution is used to determine the concentration of
an unknown solution. The component whose concentration is to be estimated is known
as titrate. Titrimetric analysis is another name for volumetric analysis.
Types of Titration
There are three different types of volumetric analysis:
1. Simple titration:
Simple titration is used to determine the concentration of an unknown solution using
the concentration of another known solution. Simple titration can be further divided
into four categories:
•Acid-base Redox Precipitation Complexometric
2. Back titration:
Back titration determines the concentration of an analyte by
reacting it with a known amount of excess reagent, whereas a
direct titration examines the concentration of an unknown
chemical directly. Excess reagents are not added in direct
titrations. Back titration is also known as indirect titration.
3. Double titrations
Apparatus used for Volumetric Analysis
The apparatus needed for volumetric analysis are as follows:
•Burette, pipette, measuring flasks, and measuring cylinders.
•Flasks for general titration, beaker, tile, glass rod, funnel, weighing
bottle, and wash bottle.
•Weighing machine with a chemical balance
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Principles of Volumetric Analysis
•An unknown amount of substance must be present in the solution which needs to be
examined.
•To show the end-point, the titrant reacts with the titrate in the presence of an
indicator. The end-point is the point at which the reaction is finished.
•The reaction between the titrant and the titrate is completed by titration which is
used to measure the volumes.
•The volume of titrant solution is obtained from the titration and concentration of
titrant used in the titration is calculated from the weight of the salt taken.
•From this we can calculate the concentration of the unknown solution.
Procedure for Volumetric Analysis
•A typical titration begins with a calibrated burette containing the titrant and a
beaker with a precise volume of the analyte with a small amount of indicator in it.
•The solution that needs to be analyzed must have a minimum amount of the material
which is needed to be analyzed.
•It's also important to choose the right kind of material to analyse because the wrong
type of titrant will give the wrong results. It is decided to use a material that reacts
quickly and thoroughly to form a complete solution.
•We can weigh and dissolve the reagent into a solution such that it is in a
defined volume within a volumetric flask.
•Since molarity is a standard measure for calculating the number of moles
present in a solution. Measuring the correct volume of the standard
solution is also important.
•Small amounts of titrant are needed to be added to the analyte and until
the indicator changes color. This will indicate that the titration has reached
its endpoint.
•The titration must be continued until the reaction is finished and the
amount of reactant introduced is exactly the amount required to finish the
reaction.
•A single drop or less than a drop of the titrant makes the difference
between a permanent and transitory alteration in the indication,
depending on the desired endpoint.
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Things to Remember based on Volumetric Analysis
•Volumetric Analysis is used to measure the concentration of a substance in a
solution by adding the same number of compounds of another substance present in
a solution of known concentration.
•The Volumetric Analysis method is also known as Titration.
•The titrant is the component whose solution is used to determine the concentration
of an unknown solution.
•The titrate is the component whose concentration is to be estimated.
•Titration is of three types: simple titration, back titration and double titration.
•A primary standard is an ultrapure compound that serves as the reference
material for a titration or for another type of quantitative analysis. A secondary
standard is a compound whose purity has been determined by chemical analysis.
•A secondary standard solution is a solution that is made specifically for a certain
analysis. A secondary standard is a substance whose active agent contents have
been found by comparison against a primary standard. This means it is usually
standardized against a primary standard.
A primary standard solution is a solution with a high purity and less
reactivity. A secondary standard is not that pure and is chemically
reactive than primary standards. This is the main difference between
primary and secondary standard solution.
What is a Primary Standard Solution
Primary standard solutions are solutions made out of primary standard
substances. A primary standard is a substance of known high purity
(99.9% pure) which may be dissolved in a known volume of solvent to
give a primary standard solution. Primary standards are reagents that can
involve in chemical reactions. These compounds are often used to
determine the unknown concentration of a solution that can undergo a
chemical reaction with the primary standard.
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Primary standards comprise special chemical and physical properties.
These compounds are extremely pure and highly stable. Therefore, we
can obtain pure solutions using these compounds. For example, if we
want to prepare a standard solution of 0.1 molL-1 concentration, we can
calculate the weight of the primary standard required for this and then
dissolve that amount in a suitable solvent. This gives exactly the 0.1
molL-1 solution with a high purity.
Primary standards are highly pure due to their low reactivity. If these
compounds were highly reactive, they could get contaminated with
many other chemicals, forming impurities. Primary standards are
less hygroscopic. Therefore they do not absorb moisture from the air in
considerable amounts. This also makes the primary standards highly
pure compounds. Eg:KBrO3, NaCl
What is a Secondary Standard Solution
A secondary standard solution is a solution that is made specifically for a
certain analysis. A secondary standard is a substance whose active agent
contents have been found by comparison against a primary standard. This
means it is usually standardized against a primary standard.
Secondary standard solutions are used to calibrate analytical equipment and
analytical techniques. These solutions do not fulfill the requirements of a
primary standard. A secondary standard has a less purity than a primary
standard. These are less stable and chemically reactive than primary
standards. Therefore these compounds can get contaminated.
Anhydrous sodium hydroxide is a secondary standard. It is highly
hygroscopic. Potassium permanganate is another compound that is often
used as a secondary standard. It is less stable and is reactive. Therefore
when a Potassium permanganate solution is being prepared, it has to be
standardized with a primary standard.
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Applications
Primary Standard Solution: Primary standard solutions are
used to standardize secondary standards and other reagents.
Secondary Standard Solution: Secondary standard solutions
are used for specific analytical experiments.
Conclusion
Standard solutions can be divided into two groups as primary
standard solutions and secondary standard solutions. Primary
standard solutions are solutions made out of primary standard
substances. Secondary standard solutions are not as pure as
primary standard solutions. Purity is the main difference
between primary and secondary standard solution.
The basic principle of the titration is the following: A solution – a so called titrant
or standard solution – is added to sample to be analyzed. The titrant contains a
known concentration of a chemical which reacts with the substance to be
determined. The titrant is added by means of a burette. The concentration of a
basic solution can be determined by titrating it with a volume of a standard acid
solution (of known concentration) required to neutralize it. The purpose of the
titration is the detection of the equivalence point, the point at which
chemically equivalent amounts of the reactants have been mixed.
The analytical method wherein the concentration of a substance in a solution
is estimated by adding exactly the same number of equivalents of another
substance present in a solution of known concentration is called volumetric
analysis.
Volumetric titration relies on getting to an equivalence point by controlled addition
of a solution of a known concentration - generally delivered from a burette - to a
known volume but unknown concentration in a conical flask. The equivalence point
for acid-base reactions is registered by use of an indicator that changes colour at
equivalence.