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Analytical Chemistry 1

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Analytical Chemistry - I

CHE 1122
Lecture - 01

A.M.K.C.J. Costa
Lecturer (Probationary)
Department of Limnology and Water Technology
Faculty of Fisheries & Marine Sciences and Technology
Recommended Text Books

Fundamentals of Analytical Chemistry, 8 th Edition, by Skoog and West


Course content
• Volumetric analysis

• Buffer solutions

• Basic statistics for chemical analysis.


Course content
Titrimetric methods
• Neutralization titrations
• Complexometric titrations
• Iodometric titrations
• Argentometric titrations
• REDOX titrations
Gravimetric methods

Statistical analysis
Learning outcomes (Lecture 1)

At the end of this lecture, students will be able to


describe:

• Quantitative analysis
• Basic analytical methods in quantitative analysis
• Volumetric titrimetric Analysis
• neutralization titrations
CHEMICAL ANALYSIS

Qualitative analysis Quantitative analysis


Quantitative analysis

• Analysis carried out to determine how much of each component is


exactly present in a mixture or in a specified component.

• Variety of techniques are available for carrying out quantitative analysis


eg: Classical method (Titrimetry, gravimetry) Instrumental methods
(Thermal methods, spectral methods)
Basic analytical methods in quantitative analysis
Gravimetric methods

• Amount of analyte can be determined through the measurement of


mass.
• Main types of gravimetric analysis:
Precipitation methods
Volatilization methods
Electro analytical methods
Basic analytical methods in quantitative analysis
Titrimetric Methods

• Contains basic and powerful methods in quantitative analysis


• This technique is based on measuring the amount of a reagent of known
concentration, that is consumed by an analyte.

• Can be classified mainly in to three groups


Volumetric titrimetry
Gravimetric titrimetry
Coulometric titrimetry
Terms used in Volumetric Titrimetry
Titration
A process in which a standard reagent is added in to a solution of an analyte until the reaction
between the reagent and the analyte is completed.

Titrant
The reagent of known concentration.(Normally the solution in the burette

Titrand
The substance being titrated
Terms used in Volumetric Titrimetry
Primary Standard
• A highly purified compound, that serves as a reference material.
• Important requirements for a primary standard:
- High purity
- Atmospheric stability
- Absence of hydrate water (composition does not change with
humidity)
- Modest cost
- Reasonable solubility in the titration medium
- Reasonably large molar mass (Errors associated with
weighing the standard is minimized)
Terms used in Volumetric Titrimetry
• Examples for primary standards

- Sodium carbonate (Na2CO3)


- Sodium tetra borate (Na2B4O7) Acid base titrations
- Potassium Hydrogen phthalate (KHP)

- Sodium oxalate (Na2C2O4)


- Potassium dichromate (K2Cr2O7) REDOX titrations
- Potassium Iodate (KIO3)
Terms used in Volumetric Titrimetry
Secondary Standard
• This is usually standardized against a primary standard.
Standard solution
Desired properties of standard solutions:
• Sufficiently stable
• React rapidly with the analyte
• React completely with the analyte
• Undergo a selective reaction with the analyte
Terms used in Volumetric Titrimetry
Standardization
• The concentration of a volumetric solution is determined by, titrating it
against a carefully measured quantity of primary or secondary standard.

Equivalence point

• Is the point in the titration, when the amount of added standard reagent
is exactly equivalent to the amount of analyte

• Equivalence point can’t be determined experimentally


Terms used in Volumetric Titrimetry

End point
Is the point in the titration, that a physical change occurs, which is
associated with the chemical equivalence.

Titration error

The difference in the volume or mass between the equivalence point


and the end point.
Indicators
• These are often added to the analyte solution to produce an
observable physical change at or near the equivalence point

• Large changes in the relative concentration of analyte or titrant occur in the


equivalence point region.

• These concentration changes cause the indicator to change its


appearance.

• Typical indicator changes include appearance or disappearance of color,


appearance or disappearance of turbidity
Introduction to neutralization titrations

• Include the titration of free bases, or those formed from salts of weak
acids by hydrolysis, with a standard acid (Acidimetry) or

• Titration of free acids or those formed by the hydrolysis of salts of weak


bases with a standard base (Alkalimetry)

• The reaction involves the combination of H+ and OH- ions to form H2O
Neutralization indicators
• In a titration, the correct end point will be characterized by a definite
value of H+ concentration of the solution, which depends on the nature
of the acid, the nature of the base and the concentration of the
solution.
• Neutralization or acid – base indicators change color according to
the H+ ion concentration of the solution
Neutralization indicators
• An acid - base indicator is a weak acid or weak base, in which the
ionized molecule has a different color from the parent molecule which
responds to a change in acidity or alkalinity by a color change

• So, these color changes are believed to be due to structural changes


occur in the molecule.

• The equilibrium between the acidic form (HIn) and the basic form
( In- ) of an indicator can be expressed as,
• An acid/base indicator is a weak organic acid or a weak organic base
whose undissociated form differs in color from its conjugate base or
its conjugate acid form.

• For example, the behavior of an acid-type indicator, HIn, is described


by the equilibrium

• The equilibrium for a base-type indicator, In, is


The equilibrium-constant expression for the dissociation of an acid-
type indicator takes the form.

[In-]
𝑝𝐻 = 𝑝𝐾 𝐼𝑛 + log
[HIn]
𝑝𝐾𝐼𝑛 = Indicator constant
•HIn, exhibits its pure acid color when

• Color change interval is:


𝑝 𝐻 = 𝑝𝐾𝐼𝑛± 1
• Within this range indicator will appear to change from one color to
another
In practice, choose an indicator whose end point lies on the steep part of the
titration curve. Because the equivalence point also lies on the steep part of
the curve, this choice ensures that the pH at the equivalence point will fall
within the range over which the indicator changes colour.

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