CHE 2101 Analytical Chemistry KAB

CHM 2101 Analytical Chemistry
By
ABUBAKAR CHADI SADIQ (PhD)

(KABALE UNIVERSITY)
Contents:
• Introduction
• The Nature of Analytical Chemistry
• Functions and applications of analytical chemistry
• A general overview of analytical techniques and Methods
• Sampling theory
• Methods of sampling
• Sample handling, storage and pre-treatment
• Standardization and calibration

Introduction
physic
al
Chemistr
Analytical
y organic
Inorganic
 Analytical Chemistry is the science of identification, obtaining,
characterizing, processing, and communicating information about
the composition and structure of matter. In other words, it is the
art and science of determining what matter is and how much of it
exists.
 Inorganic Chemistry is concerned with the properties and

behavior of inorganic compounds, which include metals, minerals,
and organometallic compounds.
 Organic Chemistry is the study of the structure, properties,

composition, reactions, and preparation of carbon-containing
compounds
 Physical Chemistry is a science that studies solid state, reaction

rate theory, kinetic theory, transport characteristics, elementary
statistical mechanics, and chemical reaction dynamics.
The Nature of Analytical Chemistry
During the 1662-1900 AD significant analytical

contributions were made by chemist such as
The development of systematic analytical analysis

by Justus von Liebig
Systematized organic analytical activities based on
the specific reactions of functional groups.
Major development of analytical chemistry started

after 1900.
During this period instrumental analysis become

progressively dominated in the field
• Analytical chemistry is a measurement science consisting of a
set of powerful ideas and methods that are useful in all fields of
science, engineering, and medicine.
• Its interdisciplinary nature stems from collaboration with other

scientific fields. For instance, in environmental science,
analytical chemistry helps assess pollution levels. In medicine,
it contributes to diagnostic tests.
• NASA's rover investigations of the planet Mars have produced

several fascinating examples of the value and strength of
analytical chemistry. These examples have happened, are
happening, and will continue to happen.
Analytical
methods
Classical Instrumental
Classical Methods
2. Gasometry
1. Volumetric Analysis
3. Gravimetric
• analysis
Aqueous acid-base titration
• 4. Karl Fischer
Non aqueous titrations
• titration
Precipitation titrations
• 5. Kjeldahl methods
Oxidation-reduction titrations
• Complexometric titrations
• Amino acid titrations
• Diazotization titrations
Instrumental
Methods
Electrochemistr Thermochemist
Spectroscopic Separation
y ry
Spectroscopi
c
Absorption and emission of light and
other radiation by matter
Nuclear Magnetic
Atomic Absorption Resonance Mass Spectroscopy
Spectroscopy (AAS) Spectroscopy (MS)
(NMR)
Absorption Fluorescence
X-ray Diffraction Spectroscopy
spectroscopy
Electrochemistry
Study of electricity and how it relates to

chemical reactions.
Potentiometric
Electrolytic
Polarography
Conductometry
Thermal methods
Differential Thermal
analysis (DTA)
Differential Scanning
Colorimetry (DSC)
Thermogravimetric
Analysis (TGA)
Separation methods
Chromatography • Gas chromatography (GC)

• High performance liquid (HPLC)
• Thin layer chromatography
• Ion exchange chromatography
Electrophoresis
• Liquid chromatography
• Paper chromatography
• Column chromatography
Extraction
OTHER METHODS OF ANALYSIS
Flame
photometr
y
Polarimet
ry
Nephelomety
and Refractometry
Turbidimery
ROLES OF ANALYTICAL CHEMIST
VOLUMETRIC METHODS OF
ANALYSIS
TITRATION
This is an analytical
method in which a
standard solution is used
to determine the
concertation of an
unknown solution
TERMS USED IN TITRATION
 Titrant: The substance added to the analyte in a titration (reagent
solution).
 Analyte a substance whose chemical constituents are being

identified and measured, e.g., in blood glucose testing, the analyte is
glucose.
 Equivalence point/stoichiometric point is the point in a

chemical reaction when there is exactly enough to complete the
reaction in the solution.
 End point: The point at which a sudden change in a physical

property of the solution occurred. This may be indicator colour,
absorbance, pH or conductivity.
 Indicator: substances that change colour when they are added to

reacting solutions. E.g., Litmus, phenolphthalein, and methyl orange
are all indicators that are commonly used in the laboratory.
 Titration error: The difference between the observed end
point and the true equivalence point in titration.
 Blank titration: a titration without an analyte being present,

only the solvent used in the analyte solution. It is carried out
like a regular titration but with no analyte present. A fixed
amount of a known concentration of titrant is added into a
solution without an analyte and results determined.
 Primary standard: A reagent which can be weighed easily,

and which is so pure that its weight is truly representative of
the number of moles of substance contained.
 Standardization: The process of determining the exact

concentration (molarity) of a solution. Concentration is
determined by reaction with known quantity of a second
reagent.
 Standard solution: Any chemical solution which has a
precisely known concentration. Its prepared by dissolving
a known mass of solute and dilute the solution to a
known volume.
 Direct titration: The typical or normal type of titration

where the standard reagent (titrant) is added to
determine the concentration of the analyte until it
reaches the endpoint.
 Back/Reverse titration: The concentration of an

analyte (unknown concentration) is determined by
reacting it with an excess amount of a known standard
reagent. The excess of standard reagent is added to react
with the analyte, then, the excess reagent is titrated with
a second reagent or with a standard solution of analyte.
SAMPLING THEORY
In any analytical procedure, there are specific

analytical method selected depends on how much
sample is available and how much analyte is
present. Selecting a particular method to be used, a
representative sample must be acquired.
Sampling: A defined procedure where a part of a

substance, material, or product is taken to provide for
testing or calibration to give a representative sample of
the bulk.
Once the analytical sample has been acquired, it

must be processed in a dependable manner that
maintains sample integrity without losing sample or
introducing contaminants.
Types of Samples and Methods
• Basically, analysis are carried out to identifying chemical

species, a qualitative analysis, from one to determine the
amount of a constituent, a quantitative analysis.
• Quantitative methods, are traditionally classified as gravimetric

methods, volumetric methods, or instrumental methods.
• qualitative analysis identifies what the chemical species is based

on the chemical and physical properties; and quantitative
analysis determines the amount or concentration of the target
substance in a sample.
• Another way to distinguish methods is based on the size of the

sample and the level of the constituents.
Classification of Samples based on size
Sample Size Type of Analysis
>0.1 g Macro
0.01 to 0.1 g Semimicro
0.0001 to 0.01 g Micro
<10-4 g Ultramicro
Classification of Samples based on Constituent
Analyte Level Type of Constituent
1 to 100% Major
0.01 (100 ppm) to 1% Minor
1 ppb to 100 ppm Trace
<1 ppb Ultratrace
Real Samples
• A portion of material selected from a larger quantity (matrix)

of material.
• The matrix can contain species with chemical properties

similar to the analyte.
• Matrix components can react with the same reagents as the

analyte, or they can cause an instrument response that is not
easily distinguished from the analyte.
• These effects interfere with the determination of the analyte.

If the interferences are caused by extraneous species in the
matrix, they are often called matrix effects.
• Such effects can be induced not only by the sample itself but
also by the reagents and solvents used to prepare the
samples for the determination.
Representative Sample
• This is the concentration of the analyte in a sample to be

analyzed to contain a good representation of its levels of the
material or system being tested.
• In other words, is the composition of the gross sample and

the laboratory sample must closely resemble the average
composition of the total mass of material to be analyzed.
• The items chosen for analysis are often called sampling

units/gross sample or sampling increments.
The Gross Sample:
• This is a miniature replica of the entire mass of

material to be analyzed. It should correspond to the
bulk material in chemical composition and in particle-
size distribution if the sample is composed of particles.
Basically, gross sample size is determined by
1. The uncertainty that can be tolerated between the composition of

the gross sample and that of the whole
2. The degree of heterogeneity of the whole, and
3. The level of particle size at which heterogeneity begins.

Statistically, the goals of the sampling process are:
 To obtain a mean analyte concentration that is an unbiased

estimate of the population mean.
 This goal can be realized only if all members of the population

have an equal probability of being included in the sample.
 To obtain a variance in the measured analyte concentration

that is an unbiased estimate of the population variance so that
valid confidence limits can be found for the mean, and various
hypothesis tests can be applied.
 This goal can be reached only if every possible sample is

equally likely to be drawn.
METHODS OF SAMPLING
• Simple random sampling: The collection of number of samples on

the best location and time
• Systematic sampling: This is a method in which a random sample,

with a fixed periodic interval, is selected from a larger population.
 The fixed periodic interval called the sampling interval, is

calculated by dividing the population size by the desired sample size.
• Stratified sampling a sampling technique where the population is

divided into groups or clusters and random samples are selected from
the cluster for analysis.
• Cluster sampling: This is a sampling technique where the population

is divided into groups or clusters and random samples are selected
from the cluster for analysis.
Sample handling, storage and pre-treatment
• Sample handling: This involve the reservation-based handling

processes are used to protect the physical and chemical properties of
the specimen.
 This can involve exposure to ultra-low temperatures to prevent

unwanted biological or chemical activity, as well as the use of
preservatives.
 Sample Storage
• Label and track samples

• Choose the right containers and materials
• Follow the storage guidelines and protocols
• Maintain the storage equipment and environment
• Handle samples with care and caution
• Review and update your sample management practices.
• The pre-treatment of a sample is a stage during which the selected
analyte is treated to remove any interfering substances.
 Still, it can also be used to concentrate the analyte.
• Standardization This is a process of determining the exact

concentration (molarity) of a solution.
 This process ensures that all procedures used in research are kept the
same.
• Calibration is defined as the process of assessment and refinement
of the accuracy and precision of a method, and particularly the
associated measuring equipment (i.e., an instrument), employed for
the quantitative determination of a sought-after analyte.
 The objective of doing calibration is to establish an experiential

liaison between the instrument response signal “y-variable” and the
reaction factors “x-variable.”

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CHM 2101 Analytical Chemistry

ABUBAKAR CHADI SADIQ (PhD)

• The Nature of Analytical Chemistry

• Functions and applications of analytical chemistry

• A general overview of analytical techniques and Methods

• Sample handling, storage and pre-treatment

• Standardization and calibration

 Inorganic Chemistry is concerned with the properties and

 Organic Chemistry is the study of the structure, properties,

 Physical Chemistry is a science that studies solid state, reaction

During the 1662-1900 AD significant analytical

The development of systematic analytical analysis

Major development of analytical chemistry started

During this period instrumental analysis become

• Its interdisciplinary nature stems from collaboration with other

• NASA's rover investigations of the planet Mars have produced

Study of electricity and how it relates to

Chromatography • Gas chromatography (GC)

 Analyte a substance whose chemical constituents are being

 Equivalence point/stoichiometric point is the point in a

 End point: The point at which a sudden change in a physical

 Indicator: substances that change colour when they are added to

 Blank titration: a titration without an analyte being present,

 Primary standard: A reagent which can be weighed easily,

 Standardization: The process of determining the exact

 Direct titration: The typical or normal type of titration

 Back/Reverse titration: The concentration of an

In any analytical procedure, there are specific

Sampling: A defined procedure where a part of a

Once the analytical sample has been acquired, it

• Basically, analysis are carried out to identifying chemical

• Quantitative methods, are traditionally classified as gravimetric

• qualitative analysis identifies what the chemical species is based

• Another way to distinguish methods is based on the size of the

Sample Size Type of Analysis

Classification of Samples based on Constituent

Analyte Level Type of Constituent

• A portion of material selected from a larger quantity (matrix)

• The matrix can contain species with chemical properties

• Matrix components can react with the same reagents as the

• These effects interfere with the determination of the analyte.

• This is the concentration of the analyte in a sample to be

• In other words, is the composition of the gross sample and

• The items chosen for analysis are often called sampling

The Gross Sample:

• This is a miniature replica of the entire mass of

1. The uncertainty that can be tolerated between the composition of

2. The degree of heterogeneity of the whole, and

3. The level of particle size at which heterogeneity begins.

 To obtain a mean analyte concentration that is an unbiased

 This goal can be realized only if all members of the population

 To obtain a variance in the measured analyte concentration

 This goal can be reached only if every possible sample is

• Simple random sampling: The collection of number of samples on

• Systematic sampling: This is a method in which a random sample,

 The fixed periodic interval called the sampling interval, is

• Stratified sampling a sampling technique where the population is

• Cluster sampling: This is a sampling technique where the population

• Sample handling: This involve the reservation-based handling