UNIT- ONE

Introduction to Analytical Chemistry

1.1 Definition of Analytical Chemistry
It is a branch of chemistry which deals with:
 Theoretical foundation; and
 Method of chemical analysis.
Steps to follow in analytical chemistry:
 Separation;
 Identification; and
 Determination of the relative amounts of the
component(s) in a sample.

1
 1.2. Role of Analytical Chemistry
 Analytical chemists work to improve existing techniques to meet
the demands of for faster, cheaper, more sensitive chemical
measurements
 It plays a vital role in many research areas in:

 Pharmacy, Biochemistry, Biology, Geology

 Medical lab
 Medicine
 Industry
 Environmental
 Food and Agriculture
 Forensic
 Archaeology
 Space science

2
Analytical chemists work to improve the reliability of
existing techniques to meet the demands of for better
chemical measurements which arise constantly in our
society
They adapt proven methodologies to new kinds of
materials or to answer new questions about their
composition.
In this regard analytical chemistry serves as an important
tool for gatheringquantitative information .
 Analytical chemistry does not just belong to chemists
only.
If you breathe the air, eat, drink, use manufactured goods,
or visit the doctor when you are ill, your life depends on 3
The Relationship Between Analytical Chemistry and The
Other Sciences

4
 continued…
Several different areas of
analytical chemistry:
1.Clinical analysis - blood, urine, faeces(body of solid waste), cellular fluids, etc., for
use in diagnosis.
2.Pharmaceutical analysis - establish the physical properties, toxicity, metabolites,
quality control, etc.
3.Environmental analysis - pollutants, soil and water analysis, pesticides.
4.Forensic analysis - analysis related to criminology; DNA finger printing, finger print
detection; blood analysis.
5.Industrial quality control - required by most companies to control product quality.
6.Bio analytical chemistry and analysis - detection and/or analysis of biological
components (i.e., proteins, DNA, RNA, carbohydrates, metabolites, etc.).

5
 1.3.Classification of Analytical Chemistry
1.Qualitative analysis :
provides information about the identity of an atomic,
molecular or biomolecular species
ions are divided in to anions and cations.
Example:- Screening athlete’s urine performance enhance
drugs.
2. Quantitative analysis :
provides numerical information as to the relative amounts of
species
* Which one is prioritized?
qualitative or quantitative analysis.
1st qualitative information
2nd quantitative analysis
Qualitative analysis is about what. Quantitative analysis is about how much.

6
 1.4. Methods of Chemical analysis
 Gravimetric Methods: Determine the mass of the analyte or
some compound chemically related to it.
 Volumetric Methods: The volume of a solution containing
sufficient reagent to react completely with the analyte is
measured.
 Spectroscopic Methods: Based on measurement of the
interaction between electromagnetic radiation and analyte
atoms or molecules.
 Chromatographic Methods: Separation techniques and
quantitation is based on calibration curve.
 Electro-analytical Methods: Involve the measurement of
electrical properties such as voltage, current, resistance
and quantity of electrical charge.

7
 Analytical Methods
Classical Methods : Wet chemical methods
such as precipitation, extraction, distillation,
boiling or melting points, gravimetric and
titrimetric measurements.
Instrumental Methods : Analytical
measurements (conductivity, electrode
potential, light absorption or emission, mass-to-
charge ratio, fluorescence etc.) are made using
instrumentation.

8
1.5. Steps in Quantitative Chemical Analysis

9
 1.5 Steps in Quantitative Chemical Analysis
1.Defining the Problem
 This step involves identification of the objectives of the problem.

 Before the analyst can design an analysis procedure, he/she

must know what information is needed, and what type of
sample is to be analyzed.

 This will dictate how the sample is to be obtained, how much is

needed, how sensitive the method must be, how accurate and
precise it must be, and what separation may be required to
eliminate interference

10
 …Continued…
2.Selecting a Method of Analysis
 A first step in quantitative analysis is the selection of a
method.
 factors that need to be considered in the selection
process are:
 The level of accuracy required
 Cost of analysis (total investment)
 Number of samples to be analyzed
 Time required for analysis
 Skill required
 Complexity of the sample as well as the number of
components in the sample.
11
 …Continued…
3.Sampling
The sample whose composition represents that of thebulk
of material from which it was taken.
 Where the bulk islarge and heterogeneous, great effort is
required to get a representative sample.
 Proper sampling is the most difficult step and the source
of greatest error.
4.Preparing a Laboratory Sample
A solid laboratory sample is:
 ground to decrease particle size,
 mixed to assure homogeneity, and
 stored for various lengths of time before the analysis
begins.
12
 …Continued…

5.Defining Replicate Samples

 Most chemical analysis are performed onreplicate samples .
 Replicate samples or replicates are portions of a material
the same size that are carried through an analytical
procedure at the same time.
 Replication improves the quality of results and provides a
measure of their reliability
 Quantitative measurements on replicates are usually
averaged, and various statistical tests are performed on the
results to establish reliability.

13
 Continued…

6.Preparing Solutions of the Samples

 Most analyses are performed on solution of the sample.
 the solvent should dissolve sample rapidly and completely.
 dissolutions should be sufficiently mild conditions.
 many materials are insoluble in common solvent.
 Conversion of the analyte in such materials into a soluble
form can be difficult and time-consuming task.
 Conversion to soluble form by
 Heating the sample with aqueous solutions of SA, SB,
oxidizing, reducing agents
 Ignition of the sample in air or oxygen; or fusion

14
 Continued…
7.Eliminating Interferences
Species other than the analyte that affect the final
measurement are called interferences.
the analyte should be eliminated from interferences before
the final measurement is made.
8.Calibration and Measurement
All analytical results depend on a final measurementX of a
physical property of the analyte.
 This property must vary in a known and reproducible way with
the concentrationC A of the analyte.
 Ideally, the measurement of the physical property is directly
proportional to the concentration. That is:CA = k X
 The process of determiningk is thus an important step in
most analyses and is termed acalibration.
15
 9.Calculating Results
 Computing analyte concentrations from experimental
data is ordinarily a simple and straightforward task,
particularly with modern calculators or computers.
 Such computations are based on the raw experimental
data collected in the measurement step, the
stoichiometry of the chemical reaction up on which the
analysis is based, and instrumental factors.
Evaluating Results from Estimating Their Reliability
 Analytical results are incomplete without an estimate of
their reliability.
 The experimenter must provide some measure of the
uncertainties associated with computed results if the
data are to have any value.
16
 1.6.Methods of Qualitative Analysis
Qualitative analysis focuses on component identification of a given unknown sample.
 It does not bother about exact quantification.
 Basically qualitative analysis can be achieved by means of variety of methods,
categorized as chemical and instrumental methods of analysis.
 Chemical methods of analysis mainly involve chemical reactions while
instrumental analysis uses special instruments.
 Instrumental methods consist of physical and physico-chemical methods of
analysis.
 In general the different methods of analysis can be categorized in to three, namely:
i. Chemical
ii. Physical and
iii. Physico - chemical methods of analysis

17
 1.6.1. Chemical methods of qualitative analysis
 The name itself indicates that this method of analysis
involves chemical reaction.
 In this method, an element or ion to be determined is
converted in to a compound having some specific properties.
 On the basis of specific properties such ascolor , solubility,
odor, etc.; one can establish the identity of the compound.
 The conversion of an element or ion into a compound having
specific properties involves a chemical change.
 This chemical change is known asanalytical reactions .
 The substance responsible for this change is called analytical
reagents .
18
1.6.2. Physical and Physico – Chemical Methods of Analysis
 The physical and physico – chemical methods are collectively named
as instrumental methods of analysis.
 They are so called since the measurement involved requires special
instrument,
i.e., the instruments measure definite parameters characterizing the
physical and/or chemical properties of a substance with high accuracy.
Examples: -
 Optical methods - depends on the color of solution substances

 Electrochemical methods - rely on measurement of electrical

properties such as potential, current, resistance, charge, etc.

 Physical methods - deal with physical properties

19
 Assignment 1
1.Define the following terms:
a. Analytical chemistry
b. Interference
2. Distinguish between or among the following:
a. Qualitative and quantitative analysis
b. Sample and analyte
3. What is meant by instrumental method of chemical analysis?
How are the physical properties used for chemical analysis?
4. In order to solve an analytical problem, a chemist has many
instrumental methods at this disposal. What factors should
be taken into consideration while selecting a given analytical
method to solve a given analytical problem?

20