Analysis

Definition of Analysis: Analytical chemistry is the

scientific study of identifying and quantifying the
composition of substances and materials. The field
encompasses a range of techniques used to determine
the chemical and physical properties of materials. Here
are some common techniques used in analytical
chemistry:
A. Qualitative analysis
• Qualitative analysis is an important tool used in analytical
chemistry to determine the presence or absence of specific
chemical constituents in a sample. This technique is useful
in identifying the type of compound or element that may
be present in a sample, but it does not provide information
on the amount of the substance present in the sample.
Qualitative analysis is typically used when the identity of a
substance needs to be determined or when the sample is
too small to measure the quantity of the substance
accurately.

• Various methods of qualitative analysis are used in

analytical chemistry, including chemical tests, flame tests,
and inorganic qualitative analysis. Each method has its own
unique advantages and limitations.
1. Chemical Tests
• Chemical tests are a common qualitative analysis method used to identify a
substance’s quality based on specific chemical reactions. These tests are typically
performed by adding a sample reagent and observing the chemical reaction. The
reaction can provide valuable information about the presence or absence of
specific chemical constituents in the sample. Some examples of chemical tests
include the acid test for gold, which is used to determine if a sample contains real
gold or a gold-plated material, and the Kastle-Meyer test for blood, which is used
to detect the presence of blood in a sample.
2. Flame Tests
• Flame tests are another common method of qualitative analysis used in analytical
chemistry. This technique involves observing the colour of flames produced by
certain elements when they are heated. Each element produces a unique colour
when heated in a flame, making it possible to identify the element based on the
colour of the flame. For example, sodium produces a bright orange-yellow flame
when heated in a flame, while copper produces a blue-green flame.
3. Inorganic qualitative analysis is a more complex method used to identify the
presence of certain ions or elements in a liquid. This method involves performing a
series of tests to identify specific ions or elements, followed by additional testing to
confirm the results. Inorganic qualitative analysis is typically used when a more
detailed sample analysis is required.
B. Quantitative analysis
• Quantitative analysis is a fundamental technique in analytical
chemistry that involves determining the amount or concentration
of specific chemical constituents in a substance. This technique
provides valuable information on the quantity of a substance
present in a sample, which is essential for various applications in
many scientific fields, including pharmaceuticals, food and
beverage, environmental monitoring, and material science. Here
are some key aspects of quantitative analysis:

1. Gravimetric analysis:
• Gravimetric analysis is a quantitative method used to determine the
weight or mass of a sample, which can then be used to calculate
the amount of a specific chemical constituent in the sample. This
method involves several steps: sample preparation, drying, and
weighing. The difference in weight before and after the experiment
determines the amount of the chemical constituent present in the
sample. Gravimetric analysis is widely used to determine
pharmaceuticals’ purity and environmental samples’ analysis.
2. Volumetric analysis
• Volumetric analysis is a quantitative method that involves the
measurement of the volume of a substance to determine its
concentration. This technique is widely used in chemical analysis and
involves using various chemical reagents to determine the concentration
of a particular chemical constituent in a sample. An example is titration,
which involves gradually adding a known amount of a reagent to the
sample until the reaction reaches its endpoint, marked by a change in
color or some other measurable property.

3. Titration is a widely used volumetric analysis technique involving an

indicator to signal the reaction’s endpoint. The indicator is a
substance that changes color when the reaction reaches its
endpoint. The choice of the indicator depends on the specific
chemical reaction being analyzed. For example, phenolphthalein is a
commonly used indicator in acid-base titrations, while potassium
permanganate is used in redox titrations.
Purpose of Quantitative analysis
1. Quantitative analysis in environmental
monitoring
• Quantitative analysis plays an essential role in
environmental monitoring, which determines the
concentration of pollutants in air, water, soil, and
other environmental samples. This technique
helps identify the sources and levels of
contamination and informs the development of
effective remediation strategies. Some common
quantitative analysis techniques used in
environmental monitoring include gas
chromatography-mass spectrometry, atomic
absorption spectroscopy, and inductively coupled
plasma mass spectrometry.
2. Quantitative analysis in pharmaceuticals
• Quantitative analysis is also an important technique in the
pharmaceutical industry, where it is used to determine the
purity, potency, and concentration of active ingredients in
drugs. This information is crucial in ensuring the safety and
efficacy of pharmaceutical products. Some common
quantitative analysis techniques used in pharmaceuticals
include high-performance liquid chromatography, gas
chromatography, and mass spectrometry.
3. Quantitative analysis in material science
• Quantitative analysis is also an essential technique in
material science, where it is used to determine materials’
chemical composition and physical properties. This
technique helps identify the properties and characteristics
of materials, inform the design of new materials, and
evaluate the quality of materials. Some common
quantitative analysis techniques in material science
include X-ray diffraction, Fourier transform infrared
spectroscopy, and scanning electron microscopy.
 ANALYSIS BY INSTRUMENTAL METHODS
Instrumental methods are essential tools in modern analytical chemistry. These highly sensitive
methods can be used to identify and quantify the components of complex mixtures or trace amounts of
substances that are difficult to detect using other techniques. Instrumental methods use specialized
instruments and techniques to measure a substance’s physical and chemical properties. Instrumental
methods are an essential part of modern analytical chemistry. These highly sensitive techniques can
identify and quantify specific compounds in a sample, determine their properties, and study their
behavior. By combining different types of instrumental methods, researchers can obtain more
comprehensive and accurate information about the composition and properties of a sample.
Instrumental methods are widely used in many scientific fields, including materials science,
pharmaceuticals, and environmental analysis.

Some of the most common instrumental methods used in analytical chemistry include:
A. Spectroscopy
Spectroscopy is a technique that involves measuring how molecules interact with electromagnetic
radiation. Spectroscopy can be used to identify the chemical composition of a sample, determine its
concentration, and study its physical properties. There are many different types of spectroscopy, each
with its own unique advantages and limitations. Some of the most commonly used spectroscopic
techniques include:
1. Infrared (IR) spectroscopy: measures the absorption or transmission of infrared radiation by a
sample, which can be used to identify functional groups and determine the composition of a sample.
2. Ultraviolet-visible (UV-Vis) spectroscopy: measures the absorption or transmission of ultraviolet and
visible light by a sample, which can be used to identify and quantify specific compounds in a sample.
3. Nuclear magnetic resonance (NMR) spectroscopy: measures the absorption of radiofrequency
radiation by nuclei in a sample, which can be used to identify a sample’s chemical structure and
composition.
4. Raman spectroscopy: measures the scattering of light by a sample, which can be used to identify a
sample’s chemical composition and structure.
5. Mass spectrometry
Mass spectrometry (MS) is a technique that involves measuring the
mass-to-charge ratio of ions produced from a sample using electric and
magnetic fields. Mass spectrometry can identify and quantify specific
compounds in a sample, determine their molecular weight, and study
their chemical properties. There are many different types of mass
spectrometry, each with its own unique advantages and limitations.
Some of the most commonly used types of mass spectrometry include:
5(i). Electrospray ionization mass spectrometry (ESI-MS): a soft
ionization technique commonly used to analyze large biomolecules
such as proteins and nucleic acids.
5(ii). Matrix-assisted laser desorption/ionization mass spectrometry
(MALDI-MS): a soft ionization technique commonly used to analyze
large biomolecules such as proteins and nucleic acids.
5(iii). Gas chromatography-mass spectrometry (GC-MS): combines gas
chromatography and mass spectrometry to separate and identify
volatile organic compounds in a sample.
5(iv). Liquid chromatography-mass spectrometry (LC-MS): combines
liquid chromatography and mass spectrometry to separate and identify
compounds in a sample.
7. Thermal analysis
• Thermal analysis is a technique that involves measuring the
interaction of a substance with heat. Thermal analysis can be used
to study a sample’s physical and chemical properties, determine its
thermal stability, and identify its composition. There are many
different types of thermal analysis, each with its own unique
advantages and limitations. Some of the most commonly used
types of thermal analysis include:
7(i). Differential scanning calorimetry (DSC): measures the difference
in heat flow between a sample and a reference material as the
temperature changes, which can be used to determine the thermal
behaviour of a sample.
7(ii). Thermogravimetric analysis (TGA): measures a sample’s weight
as the temperature changes, which can be used to determine a
sample’s thermal stability and composition.
7(iii). Dynamic mechanical analysis (DMA): measures a sample’s
mechanical properties as the temperature changes, which can be used
to study the viscoelastic behaviour of materials.
B. Separation techniques
• Separation techniques are an essential tool in
analytical chemistry. They enable researchers
to isolate and identify individual components
in a mixture, making it possible to quantify the
concentration of each component. Separation
techniques are used in many fields, including
pharmaceuticals, food science, environmental
analysis, and materials science.
• There are several types of separation techniques, each with its own
advantages and limitations. Here are some of the most common
separation techniques used in analytical chemistry:
1. Chromatography
• Chromatography is a technique used to separate compounds based on
their chemical properties and their ability to interact with a stationary
phase. The stationary phase can be a solid or liquid material immobilized
on a column or a plate. The sample is introduced to the column or plate,
and the components in the sample separate based on their interactions
with the stationary phase. The different types of chromatography include:
(i). Gas chromatography (GC): Separates compounds based on their volatility
and interactions with a stationary phase.
(ii). Liquid chromatography (LC): Separates compounds based on their
polarity and interactions with a stationary phase.
(iii). High-performance liquid chromatography (HPLC): Similar to LC, but with
higher resolution and faster analysis times.
(iv). Thin-layer chromatography (TLC): Separates compounds based on their
polarity and interactions with a stationary phase on a thin material layer.
2. Electrophoresis
• Electrophoresis is a technique used to separate molecules based on their size and
charge. The sample is introduced to a gel matrix, and an electric field is applied to
the gel. The molecules in the sample move through the gel matrix based on their
size and charge, resulting in bands of separated molecules. The different types of
electrophoresis include:
2(i). Gel electrophoresis: Separates molecules such as DNA, RNA, and proteins based
on size and charge.
2(ii). Capillary electrophoresis: Similar to gel electrophoresis, but with higher
resolution and faster analysis times.

3. Field flow fractionation

• Field flow fractionation is a technique used to separate particles based on their
size, shape, and density. The sample is introduced to a flow field, and the particles
move through it based on their physical properties. The different types of field
flow fractionation include:
3 (i) Asymmetric flow field flow fractionation (AF4): Separates particles based on size
and shape.
3(ii) Centrifugal field flow fractionation (CFFF): Separates particles based on size and
density.
4. Hybrid techniques
Hybrid techniques in analytical chemistry involve combining multiple analytical techniques to enhance
the accuracy and precision of the analysis. These techniques are commonly used in complex
analysis situations where one technique alone may not provide all the necessary information.
Hybrid techniques have revolutionized analytical chemistry and made it possible to identify and
quantify trace amounts of substances in a sample with greater accuracy and sensitivity.
There are various hybrid techniques, but two of the most common are gas chromatography-mass
spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS).
4(i). Gas chromatography-mass spectrometry (GC-MS)
GC-MS is a hybrid analytical technique that combines gas chromatography (GC) and mass
spectrometry (MS) to separate and identify compounds in a sample. Gas chromatography
separates a mixture of compounds based on their boiling points, while mass spectrometry
identifies the compounds based on their mass-to-charge ratio. This technique has become the
gold standard for forensic drug analysis and is used widely in the pharmaceutical industry to
analyze drug impurities.
The GC-MS process involves the following steps:
The sample is introduced into the gas chromatograph, vaporized and separated into its component
parts.
The separated compounds are then ionized and fragmented by the mass spectrometer.
The resulting ions are then separated and detected by the mass spectrometer, which generates a
mass spectrum that provides information on the identity and quantity of the components in the
sample.
Advantages of GC-MS:
High sensitivity and specificity for detecting trace amounts of compounds.
The ability to identify and quantify multiple components in a single sample.
Compatibility with a wide range of compounds, including volatile and non-volatile substances.
4(ii). Liquid chromatography-mass spectrometry (LC-MS)
LC-MS is another hybrid analytical technique that combines liquid
chromatography (LC) and mass spectrometry (MS) to identify and quantify
the components in a sample. Liquid chromatography separates a mixture
of compounds based on their polarity, while mass spectrometry identifies
the compounds based on their mass-to-charge ratio. This technique is
widely used in the pharmaceutical industry to analyze drug metabolites,
protein analysis, and environmental monitoring.
The LC-MS process involves the following steps:
The sample is introduced into the liquid chromatograph and separated into
component parts based on their polarity.
The separated compounds are then ionized and fragmented by the mass
spectrometer.
The resulting ions are then separated and detected by the mass
spectrometer, which generates a mass spectrum that provides information
on the identity and quantity of the components in the sample.
Advantages of LC-MS:
High sensitivity and specificity for detecting trace amounts of compounds.
The ability to identify and quantify multiple components in a single sample.
Compatibility with a wide range of compounds, including polar and non-polar
substances.
Other hybrid techniques
• Other hybrid techniques used in analytical chemistry include:
• Liquid chromatography-nuclear magnetic resonance spectroscopy (LC-NMR)
• Gas chromatography-infrared spectroscopy (GC-IR)
• Capillary electrophoresis-mass spectrometry (CE-MS)
• Gas chromatography-atomic emission spectroscopy (GC-AES)
• High-performance liquid chromatography-ultraviolet-visible spectroscopy (HPLC-UV)

5. Microscopy
Microscopy is a technique used to visualize materials at a microscopic level, allowing for the observation
of their structure and properties. Analytical chemists use microscopy to study and analyze the
composition of materials and substances, including single molecules, cells, and nanomaterials. Several
types of microscopy techniques are used in analytical chemistry, including optical, electron, and
scanning probe microscopy.
5 (A) Optical Microscopy: Optical microscopy is a technique that uses visible light to observe materials
at a microscopic level. This technique is useful for studying materials’ morphology, structure, and
chemical composition. Optical microscopy can be performed using different types of microscopes, such
as bright-field microscopy, dark-field microscopy, and fluorescence microscopy. These microscopes use
different lighting and imaging techniques to observe materials differently.
5(B) Bright-field microscopy: is a standard technique that uses visible light to illuminate the sample,
producing a bright background and dark specimen. It is useful in observing the morphology and
structure of materials.
5 (C) Dark-field microscopy: is a technique that uses oblique lighting to observe materials that are
difficult to see with bright-field microscopy. It is useful in observing materials that are transparent or
have low contrast.
5 (D) Fluorescence microscopy: is a technique that uses fluorescent dyes to label specific sample
components. When illuminated with light of a specific wavelength, the labelled components emit light
of a different wavelength, allowing for their visualization.
6. Electron Microscopy
Electron microscopy is a technique that uses a beam of electrons to observe
materials at a microscopic level. This technique provides higher resolution
than optical microscopy, allowing for observing smaller structures and
features. Electron microscopy can be performed using different
microscopes, such as transmission electron microscopy (TEM) and
scanning electron microscopy (SEM). These microscopes use different
imaging techniques to observe materials at different magnification levels.
6(A). Transmission electron microscopy: is a technique that uses a beam of
electrons to observe the internal structure of materials. It provides high
resolution and allows for observing atomic and molecular structures.
6(B). Scanning electron microscopy: is a technique that uses a beam of
electrons to scan the surface of a material, producing a three-dimensional
image. It helps study the morphology and topography of materials.
6(C) Scanning Probe Microscopy: Scanning probe microscopy is a technique
that uses a probe to scan the surface of a material, providing high-resolution
images of the material’s surface. This technique includes atomic force
microscopy (AFM), scanning tunnelling microscopy (STM), and scanning
electrochemical microscopy (SECM). These techniques are useful for
observing materials’ topography and chemical properties at a nanometer
scale.
6(D) Atomic force microscopy: is a technique that uses a probe to scan the surface of a material,
measuring the forces between the probe and the material’s surface. It provides high-resolution
images of the material’s surface topography.
6(E) Scanning tunnelling microscopy: This technique uses a probe to scan the surface of a
material, measuring the tunnelling current between the probe and the material’s surface. It
provides high-resolution images of the material’s surface topography and electronic properties.
6(F) Scanning electrochemical microscopy: This technique uses a probe to scan the surface of a
material, measuring the local electrochemical reactions between the probe and the material’s
surface. It provides high-resolution images of the material’s surface topography and chemical
properties.
List of chemical analysis methods
1. Atomic absorption spectroscopy (AAS)
2. Atomic emission spectroscopy (AES)
3. Atomic fluorescence spectroscopy (AFS)
4. Alpha particle X-ray spectrometer (APXS)
5. Capillary electrophoresis (CE)
6. Chromatography
7. Colorimetry
8. Computed tomography
9. Cyclic Voltammetry (CV)
10. Differential scanning calorimetry (DSC)
11. Electrodialysis
12. Electrolysis
13. Electron microscopy
14. Electron paramagnetic resonance (EPR) also called
Electron spin resonance (ESR)
15. Electrophoresis
16. Energy Dispersive Spectroscopy (EDS/EDX)
17. Field flow fractionation (FFF)
18. Flow injection analysis (FIA)
19. Fourier transform infrared spectroscopy (FTIR)
20. Gas chromatography (GC)
21. Gas chromatography-mass spectrometry (GC-MS)
22. Gas chromatography-IR spectroscopy (GC-IR)
23. Gel permeation chromatography-IR
spectroscopy (GPC-IR)
24. High performance liquid chromatography (HPLC)
25. High performance liquid chromatography-IR
spectroscopy (HPLC-IR)
26. Ion Microprobe (IM)
27. Inductively coupled plasma (ICP)
28. Ion-mobility spectrometry (IMS)
29. Ion selective electrode (ISE) e.g. determination of pH
30. Laser induced breakdown spectroscopy (LIBS)
31. Liquid chromatography-IR spectroscopy (LC-IR)
32. Liquid chromatography-mass spectrometry (LC-MS)
33. Mass spectrometry (MS)
34. Mössbauer spectroscopy
35. Neutron activation analysis
36. Nuclear magnetic resonance (NMR)
37. Optical microscopy
38. Optical emission spectroscopy
39. Optical rotation (OR)
40. Particle induced X-ray emission spectroscopy (PIXE)
41. Pyrolysis gas chromatography mass spectrometry (PY-
GC-MS)
42. Particle size determination by laser diffraction (PSD)
43. Raman spectroscopy
44. Refractive index
45. Resonance enhanced multiphoton ionization (REMPI)
46. Secondary ion mass spectrometry
47. Supercritical fluid chromatography (SFC)
48. Transmission electron microscopy (TEM)
49. Titration
50. Thermogravimetric Analysis (TGA)
51. Vacuum fusion
52. X-ray photoelectron spectroscopy (XPS)
53. X-ray diffraction (XRD)
54. X-ray fluorescence spectroscopy (XRF)
55. X-ray microscopy (XRM)