Chapter 1

Analytical Separation Techniques and Classical Method of Analysis

Brainstorming:

Can you list some classifications of Analytical techniques/methods?

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 Analytical techniques can be catacorized into:
1. Qualitative or Quantitative
2. Classical/non-instrumental or Instrumental
 Qualitative Analysis: Focuses on identifying the components or species present in a sample.
 Quantitative Analysis: Aims to determine the numerical amount or concentration of a specific
component in a sample.

 Classical Methods:
• These techniques often involve chemical reactions, color
changes, and measuring physical changes like mass or volume.
• Examples include precipitation, extraction, distillation, and
volumetric analysis.
• Stoichiometry is used for quantitative analysis using classical
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techniques,
  Instrumental Methods:
• In the 19th century, chemists began to exploit instrumental methods for solving analytical
problems.
• These techniques use sophisticated instruments to measure physical properties that relate to the analyte's concentration or identity.

Example
 Chromatography: separates components in a mixture, and also used for quantitative analysis.
 Electroanalytical methods: measure electrical properties like potential or current to analyze samples.
 Spectroscopy: measures the interaction of electromagnetic radiation with the sample.
 Mass spectrometry: measures the mass-to-charge ratio of ions to identify and quantify substances.

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 Instrumental

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  The stimulus usually in the form of electromagnetic,
electrical or mechanical energy
 Response (detector) that converts changes in properties of the
analyte to a number that is proportional to the relevant
chemical or physical absorption by the analyst.
 The detection system converts information to electrical
signals by photodiodes, photomultipliers, - etc.
 Then the electrical signal converts information to numeric or
graphic output of a photographic plat, recording paper, or
computers.
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 Advantage and disadvantages of instrumental and
classical techniques
Acuracy and precision
Sensetivity and selectivity of the method
The cost of analysis
Speed of analysis
 Sensitivity refers to the minimum amount of analyte that can
be detected or quantified by an analytical method
 Selectivity is the ability to differentiate between the analyte
of interest and other components in the sample matrix
 Speed refers to the time required for sample preparation,
analysis, and data processing
 Cost considerations include the initial investment in
instrumentation, maintenance, consumables, and operator
training

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 Advantage and disadvantages

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 Advantage and disadvantages

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 Advantage and disadvantages

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 Advantage and disadvantages

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 Advantage and disadvantages
Classical methods are most useful for
accurate and precise measurements of
analyte concentrations at the 0.1% level or
higher.
On the other hand, some specialized
instrumental techniques are capable of
detecting individual atoms or molecules in
a sample.
Analysis at the ppm (µg/mL) and even ppb
(ng/mL) level is routine for instrumental
methods.

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 Separation Techniques
Analytical separation techniques are critical in
chemistry for isolating components of a mixture.
They enable precise analysis and identification of
individual substances, enhancing the understanding
of complex samples.
Separations are carried out based on differences in
chemical properties or physical properties such as
size, shape, mass, density, magnetic properties, or
chemical affinity, between the constituents of a
mixture.
Applications: These techniques are widely utilized in

pharmaceuticals, environmental monitoring, and food

safety testing for both qualitative and quantitative
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analysis.
 Separation
Can you list the different separation techniques?
Various types of separation processes are:

Crystallization, Filtration, Decantation, Sublimation,

Evaporation, Simple distillation, Fractional distillation,
Centrifugation, Separating funnel, Magnetic separation,
Precipitation, Extraction and Chromatography.
Filtration

This is a more common method of separating an insoluble

solid from a liquid.

An example of such a mixture is sand and water.

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 Separation
 Evaporation

• Evaporation is great for separating a mixture (solution) of a

soluble solid and a solvent.

• The process involves heating the solution until the solvent

evaporates (turns into gas) leaving behind the solid residue.

 Separating funnel

• In this technique, two liquids that do not dissolve very well in

each other (immiscible liquids) can be separated by taking

advantage of their unequal density.
• A mixture of oil and water, for example, can be separated by
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 Separation

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 Separation
 Simple distillation:
• It is a method used for the separation of components of a mixture
containing two miscible liquids that boil without decomposition
and have sufficient difference in their boiling points.
• Used for a mixture in which the boiling point of the components
differ by at least 158°F (70°C).
Example: separation of acetone and water, distillation of alcohol etc.

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 Separation
 Fractional distillation: it is used for the separation of a

mixture of two or more miscible liquids for which the

difference in boiling points is less than 77°F (25°C).
• The apparatus for fractional distillation is similar to that of

simple distillation, except that a fractionating column is fitted

in between the distillation flask and the condenser.
• A simple fractionating column is a tube packed with glass

beads.
• The beads provide surface for the vapors to cool and
condense repeatedly.
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 Separation

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 Separation
Steam Distillation
 it is used for the purification of mixtures in
which the components are temperature or heat
sensitive; for eg. organic compounds.
 In this process, steam is introduced to the
apparatus and the temperature of the
compounds are depressed, by vaporizing them
at lower temperature.
The vapors are collected and condensed in the
same way as other distillation types.

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 Separation

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 Sublimation

The technique relies on heating the mixture to turn the substance

into a gas, which is then collected as a solid on a cooler surface.

 Used to separat iodine, camphor (C₁₀H₁₆O), ammonium

chloride, and naphthalene.

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 Crystallization
It separates a soluble solid from a liquid by

exploiting its temperature-dependent solubility.

The principle is that a solution is first heated to

become saturated, then cooled to become

supersaturated.
As the solution cools, the solute's solubility
decreases, causing it to precipitate out as
crystals, which can then be separated from the

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remaining liquid.
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 Common physical process used for separation

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 Separation
 Centrifugation:
It is the process of separation of tiny solid
particles that normally pass through filter paper.
It is based on the size, shape, and density of the
particles, viscosity of the medium, and the speed
of rotation.

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 Separation
 Extraction Techniques
It is a separation process consisting in the
separation of a substance from a matrix.
 It includes Liquid-liquid extraction, and Solid
phase extraction.
 liquid–liquid extraction the analyte and
interferent are initially present in a single liquid
phase.
We add a second, immiscible liquid phase and
mix them thoroughly by shaking.
During this process the analyte and interferents
partition themselves between the two phases to
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different extents, effecting their separation.
 Separation
The purpose of an extraction technique is physically to
separate components of a mixture (solutes) by exploiting
differences in their relative solubility in two immiscible liquids
or between their affinities for a solid sorbent.
 An equilibrium distribution of the solutes between the two phases is
established by dissolving the sample in a suitable solvent, then
shaking the solution with a second, immiscible, solvent or by passing
it through a sorbent bed or disk.
 Where the equilibrium distributions of two solutes differ, separation
is possible.
 The principal factors that determine how a solute will distribute
between two phases are its polarity and the polarities of each phase.
 Degree of ionization, hydrogen bonding and other electrostatic
interactions also play a part.

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 Separation

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 Separation
Digestion
It is a crucial pre-treatment step for elemental or
chemical analysis of metals.
Break down of the sample matrix to release
target analytes into a liquid form suitable for
instrumental analysis.
Common methods include traditional open-vessel
acid digestions, closed-vessel microwave
digestions, and dry ashing.
Microwave digestion is favored for its speed,
efficiency, and ability to handle a wide range of
samples with good recovery.

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 Separation
Chromatography
It is a highly efficient techniques for the separation of
components of complex mixtures prior to their qualitative
and quantitative determination.
Extraction primarily focuses on selectively pulling out specific

components from a complex mixture, often using two immiscible

liquid phases.
In contrast, chromatography is a broader technique that
separates mixtures into their individual components based on
their differential affinities for a stationary phase, driven by a
miscible mobile phase that carries the compounds through
the
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 Chromatography
Extraction can be a single step to isolate a target compound,

whereas chromatography is a more refined process for

achieving high-purity separation of multiple compounds.

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 Exercis
1. Identify the method/s can be used to separate the following mixtures
iron and copper fillings

butter from curd

isopropyl alcohol and water

Water and petrol

grains/sand/rice from chaff/husk

common salt from its solution

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 2. What is/are the basic properties used for
separations of mixtures in the following
techniques?
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