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Chapter 1_The Nature of Analytical Chemistry

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28 views31 pages

Chapter 1_The Nature of Analytical Chemistry

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Drexl Baga
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© © All Rights Reserved
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ANALYTICAL

CHEMISTRY
WHAT IS ANALYTICAL
CHEMISTRY?
Analytical chemistry is the study of
the separation, identification ,
and quantification of
the chemical components of natural and
artificial materials.
WHAT IS ANALYTICAL
CHEMISTRY?
Analytical chemistry is often described
as the area of chemistry responsible for
characterizing the composition of matter,
both qualitatively (what is present) and
quantitatively (how much is present).
WHAT IS ANALYTICAL
CHEMISTRY?
A branch of chemistry that deals with the development
and use of techniques for chemical measurement.

These techniques are used in analyzing the chemical


composition of substances. Chemical analysis may be
qualitative or quantitative.
TYPES OF ANALYSIS
Qualitative analysis reveals the
identity of the elements and compounds in a
sample.
 gives an indication of the identity of the
chemical species in the sample
TYPES OF ANALYSIS
involves attempting to identify what
materials are present in a sample. Answering the
question: "What is it?"
 Wet chemistry (precipitation, extraction and
distillation)
 Chemical tests
 Analysis of cations
 Analysis of anions
 Flame tests
TYPES OF ANALYSIS
indicates the amount of each
substance in a sample. Analytes are the
components of a sample that are to be
determined.
Quantitative analysis determines the amount of
one or more of these components. The separation
of components is often performed prior to
analysis.
The Role of
Analytical Chemistry
• Analytical
chemistry plays
a role in a wide
range of
scientific
disciplines.
 Drugs and pharmaceutical
(pharmaceutical Analysis)
 Clinical Laboratories (biological
Analysis)
 Forensic Medicine ( & crime analysis)
 Chemicals and cosmetics
 Environmental Analysis
 Research area in pharmacy, chemistry
biochemistry and biology etc.
• Blood analysis - use to diagnose and treat illness.
• To assess the effectiveness of smog-control
devices.
• Quantitative determination of elements in food
and their nutritional value.
• Analysis of steel during production permits the
adjustments in the concentrations to achieve a
desired strength, hardness, corrosion resistance,
and ductility.
• Ethyl Mercaptan content is monitored to warn for
dangerous leaks.
• Farmers - quantitative analysis of plants and
soils.
• Research - quantitative measurements of
ions in the body fluids of animals to study the
role of this ions in nerve signal conduction as
well as muscle construction and relaxation.
– Archaeologists - measuring the concentrations of
elements in samples taken in various locations.
– Medical technologists - identifications of variants
of Covid -19 present in liquid samples.
CHEMISTRY - “the central science”

• The inter-disciplinary nature of


chemical analysis makes it vital tool in
medical, industrial, government, and
academic laboratories throughout the
world.
Quantitative Analytical Methods
• A variety of analytical methods may be used.
 Gravimetric methods determine the mass of the analyte
or some compound chemically related to it.
 Volumetric methods measure the volume of a solution
containing sufficient reagent to react completely with the
analyte.
 Electroanalytical methods measure electrical properties
such as potential, current, resistance, and quantity of
electrical charge.
Quantitative Analytical Methods
• Spectroscopic methods are based on measurement of
the interaction between electromagnetic radiation and
analyte atoms or molecules or on the production of such
radiation by analytes.
– Miscellaneous methods to measure mass to charge ratio of
molecules:
• mass spectrometry, rate of radioactive decay, heat of
reaction, rate of reaction, sample thermal conductivity,
optical activity, and refractive index.
Quantitative
Analysis
1. CHOOSING A METHOD
STEPS in any quantitative analysis:
1st- The selection of the method.
Requires: experience and intuition.
2nd- the number of samples that will be analyzed...
economic factors.
3rd- the complexity of the sample
4th- the number of components in the sample
2. ACQUIRING THE SAMPLE
After selecting a method for analysis, the second step is to acquire the sample.

• Sampling is the process of collecting a small mass of a material whose


composition accurately represents the bulk of the material being sampled.
• A material is heterogeneous if its constituent parts can be distinguished visually or
with the aid of a microscope.

• It is difficult to obtain a representative sample from a heterogenous sample.

• An assay is the process of determining how much of a given sample is the


material by its indicated name.

• Note that we analyze samples and we determine substances.


2. ACQUIRING THE SAMPLE
Analysis of sample of the same composition.
– but, if it is large and heterogeneous - Ag ore
• Assay - 1.0 g - accurately represents - 23,000,000g of bulk
sample.
– Sampling - is the process of collecting a small mass of a material
whose composition accurately represents the bulk of the material
being sampled.
– Biological sources - determination of blood gases - O2 and CO2
» procedures : sampling and transporting specimens to the
Clinical laboratory.
Laboratory sample is Representative of the whole.
3. PROCESSING THE SAMPLE
•Not all samples require processing.
•Solid laboratory samples are ground, mixed, and stored.
• Drying samples prior to analysis is recommended because
loss or gain of water changes the chemical composition of
solids.
• Alternatively, a separate analytical procedure can be used to
determine the moisture content of the sample at the time of
the analysis.
3. PROCESSING THE SAMPLE
•Liquid samples can undergo evaporation of the solvent
and/or contamination by atmospheric gases.
•Two approaches can help to preserve the integrity of the
liquid sample:
• Keeping the sample container in a second sealed container.
• Manipulating and measuring the sample in an inert
atmosphere.
3. PROCESSING THE SAMPLE
•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.
• Replication improves the quality of the
results and provides a measure of their
reliability that can be established using
statistical testing.
3. PROCESSING THE SAMPLE
•Most analyses are performed on solutions of the sample made with a
suitable solvent.
•Consider whether the sample has a property proportional to the
analyte concentration that can be measured.
•If not, convert the analyte to form suitable for the measurement step.
This step may require the use of fluxes to perform the conversion.
• A flux is a material, often an alkali metal salt, that is mixed with the
sample and heated to form a fused salt.
•Before proceeding to the measurement step, eliminate interference
in the sample.
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.
•Analytes must be isolated from interferents
before measurements are made.
5. CALIBRATING AND MEASURING
CONCENTRATION
•Ideally, the final measurement X of a physical or
chemical property of the analyte is directly proportional
to the concentration of the analyte.
5. CALIBRATING AND MEASURING
CONCENTRATION
•The matrix, or sample matrix, is the collection of all the
components in the sample containing an analyte.

•Techniques or reactions that work for only one analyte are specific.
Techniques or reactions that apply to only a few analytes are
selective.

•Calibration is the process of determining the proportionality


between analyte concentration and a measured quantity.
6. CALCULATING RESULTS
•After the concentration has been calibrated and
measured, it can be calculated. These computations
are based on:
• The raw experimental data.
• The characteristics of the measurement instruments.
• The stoichiometry of the analytical reaction.
7. EVALUATING RESULTS BY
ESTIMATING RELIABILITY
•Analytical results are complete only when
their reliability has been estimated.
•An analytical result without an estimate of
reliability is of no value.
An Integral Role for Chemical
Analysis: Feedback Control Systems

•A feedback system is a process of


continuous measurement and control.
•A feedback loop is a cycle of
measurement, comparison, and control.
Feedback System Flow Diagram
REFERENCES:

oAnalytical Chemistry by Skoog, et. al.


oQualitative Chemistry by Gilreath
oChemistry by Silberberg
oChemistry Central Science by Brown,
et. al.
oGeneral Chemistry by Hein, et. al.
oGeneral Chemistry by Masterton

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