Introduction
to
Analytical
Chemistry
Prepared by:
JOSEPHINE P. BARIUAN
Instructor 1
Analytical
Chemistry
- is a measurement of
science consisting of
set of powerful ideas
and methods that are
useful in all fields of
sciences, engineering
and medicine
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Analytical
Chemistry
-studies and uses
instruments and methods
used to separate, identify,
and quantify matter. In
practice, separation,
identification or
quantification may
constitute the entire
analysis or be combined
with another method. 3
History of
Analytical
Chemistry
Significant contributions to analytical
chemistry include the development of
systematic elemental analysis by Justus von
Liebig and systematized organic analysis
based on the specific reactions of
functional groups.
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History of Analytical
Chemistry
The first instrumental analysis was flame
emissive spectrometry developed by Robert
Bunsen and Gustav Kirchhoff who discovered
rubidium (Rb) and caesium (Cs) in 1860.
The Bunsen-Kirchhoff Spectroscope with
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Bunsen Burner
History of Analytical
Chemistry
The separation sciences follow a similar time-
line of development and also become
increasingly transformed into high performance
instruments.
In the 1970s many of these techniques began to
be used together as hybrid techniques to
achieve a complete characterization of samples.
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History of Analytical
Chemistry
Lasers have been increasingly used in
chemistry as probes and even to initiate and
influence a wide variety of reactions.
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History of Analytical
Chemistry
The late 20th century also saw an expansion
of the application of analytical chemistry
from somewhat academic chemical
questions to forensic, environmental,
industrial and medical questions, such as in
histology.
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History of Analytical
Chemistry
The discovery of a chemical present in blood
that increases the risk of cancer would be a
discovery that an analytical chemist might be
involved in.
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History of Analytical
Chemistry
An effort to develop a new method might
involve the use of a tunable laser to increase
the specificity and sensitivity of a
spectrometric method.
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Nature of Analytical
Chemistry
❖ Analytical chemistry plays an increasingly
important role in the pharmaceutical
industry where, aside from QA, it is used
in discovery of new drug candidates and
in clinical applications where
understanding the interactions between
the drug and the patient are critical.
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Nature of Analytical
Chemistry
➢ A qualitative analysis determines the
presence or absence of a particular
compound, but not the mass or
concentration.
➢ By definition, qualitative analyses do not
measure quantity.
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Nature of Analytical
Chemistry
Two types of Qualitative Analysis:
❑ Chemical Test
❑ Flame test
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Nature of Analytical
Chemistry
Chemical testing might have a variety of
purposes, such as:
• Determine the interactions of a sample
with other known substances
• Determine the composition of a sample
• Provide standard data for other scientific,
medical, and Quality assurance functions
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Nature of Analytical
Chemistry
✓ A flame test is an analytic procedure used
in chemistry to detect the presence of
certain elements, primarily metal ions,
based on each element's characteristic
emission spectrum.
✓ The color of flames in general also
depends on temperature.
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Nature of Analytical
Chemistry
The color of flames in general also depends
on temperature.
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Nature of Analytical
Chemistry
Quantitative analysis is the
measurement of the quantities of
particular chemical constituents present
in a substance.
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Nature of Analytical
Chemistry
Two types of Quantitative analysis:
• Gravimetric analysis
• Volumetric analysis
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Nature of Analytical
Chemistry
Gravimetric analysis involves determining
the amount of material present by weighing
the sample before and/or after some
transformation.
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Nature of Analytical
Chemistry
Titration involves the addition of a reactant
to a solution being analyzed until some
equivalence point is reached.
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The Role of Analytical
Chemistry
Applications:
❖Determination of the concentration of oxygen
and carbon dioxide
❖Measurement of the quantities of hydrocarbons,
nitrogen oxides, and carbon monoxide present in
automobile exhaust gases
❖Quantitative measurements of ionized calcium
in blood serum
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The Role of Analytical
Chemistry
Applications:
❖Quantitative determination of nitrogen in
food
❖Analysis of steel
❖Monitor the mercaptan content of
household gas supplies
❖Tailor fertilization and irrigation schedules
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The Role of Analytical
Chemistry
Applications:
➢ Quantitative measurements of potassium,
calcium, and sodium ions in the body
fluids of animals
➢ Mechanism of chemical reactions
➢ Quantitative analysis of crystalline
germanium
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The Role of Analytical
Chemistry
Figure 1-1
The relationship between
analytical chemistry, other
branches of chemistry,
and the other sciences.
The central location of
analytical chemistry in the
diagram signifies its
importance and the
breadth of its interactions
with many other
disciplines.
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Quantitative Analytical
Methods
There are two main measurements:
1.mass or the volume of sample being
analyzed
2.some quantity proportional to the
amount of analyte such as mass, volume,
intensity of light, or electrical charge.
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Quantitative
Analytical Methods
➢Gravimetric methods: the mass of the
analyte or some compound chemically
related to it is determined.
➢Volumetric methods: the volume of a
solution containing sufficient reagent to
react completely with the analyte is
measured. 26
Quantitative
Analytical Methods
➢Electroanalytical methods: electrical
properties such as potential, current,
resistance, and quantity of electrical charge
are measured.
➢Spectroscopic methods: the interaction
between electromagnetic radiation and
analyte atoms or molecules or the emission
of radiation by analytes is explored.
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A typical quantitative
analysis
Figure 1-2 Flow diagram showing
the steps in a quantitative analysis.
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A typical quantitative
analysis
Step 1: Choosing a Method
- It requires experience as well as intuition
- Number of samples analyzed
- Complexity of the sample and the
number of components in the sample
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A typical quantitative
analysis
Step 2: Acquiring the Sample
❑ A material is heterogeneous if its
constituent parts can be distinguished
visually or with aid of a microscope.
❑ Coal, animal tissue, and soil are
heterogeneous.
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A typical quantitative
analysis
Step 2: Acquiring the Sample
❑ An assay is the process of determining
how much of a given sample is the
material by its indicated name.
❑ Zinc alloy is assayed for its zinc content,
and its assay is a particular numerical
value. 31
A typical quantitative
analysis
Step 2: Acquiring the Sample
❑ Sampling is a process of collecting a small
mass of material whose composition
accurately represents the bulk of the
material being sampled.
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A typical quantitative
analysis
Step 2: Acquiring the Sample
❑ Analyze samples and determine
substances.
❑ Blood sample is analyzed to determine
the concentrations of various substances
such as blood gases and glucose, not the
analysis of blood gases or glucose. 33
A typical quantitative
analysis
Step 3: Processing the Sample
❑ 1. Preparing a Laboratory sample
For solids, it is a good idea it is a good idea
to dry samples just before starting an
analysis.
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A typical quantitative
analysis
Step 3: Processing the Sample
❑ 1. Preparing a Laboratory sample
If liquid samples are allowed to stand in
open containers, the solvent may evaporate
and change the concentration of the
analyte.
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A typical quantitative
analysis
Step 3: Processing the Sample
❑ 1. Preparing a Laboratory sample
If the analyte is a gas dissolved in a liquid,
the sample container must be kept in a
second sealed container to prevent
contamination by atmospheric gases.
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A typical quantitative
analysis
Step 3: Processing the Sample
❑ 2. Defining Replicate Samples
Replicate samples, or replicates, are
portions of a material of approximately the
same size that are carried through an
analytical procedure at the same time and in
the same way.
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A typical quantitative
analysis
Step 3: Processing the Sample
❑ 3. Preparing Solutions: Physical and
Chemical Changes
Ideally, the solvent should dissolve the
entire sample, including the analyte, rapidly
and completely.
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A typical quantitative
analysis
Step 3: Processing
the Sample
Figure 1-2 Flow diagram showing
the steps in a quantitative analysis.
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A typical quantitative
analysis
Step 3: Processing
the Sample
Figure 1-2 Flow diagram showing
the steps in a quantitative analysis.
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A typical quantitative
analysis
Step 4: Eliminating Interferences
An interference or interferent is a species
that causes an error in an analysis by
enhancing or attenuating (making smaller)
the quantity being measured.
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A typical quantitative
analysis
Step 5: Calibrating and Measuring
Concentration
Calibration is the process of determining
the proportionality between analyte
concentration and a measured quantity.
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A typical quantitative
analysis
Step 6: Calculating Results
Computations are based on the raw
experimental data collected in the
measurement step, the characteristics of
the measurements, and the stoichiometry
of the analytical reaction.
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A typical quantitative
analysis
Step 7: Evaluating Results by Estimating
Reliablity
➢ An analytical result without an estimate
of reliability is of NO VALUE.
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