Unit 1: Analytical Techniques for Engineers

Role of Materials in Engineering Fields:

Materials play a crucial role in engineering fields, including:

1. Structural integrity: Materials provide the strength, durability, and resistance needed for
buildings, bridges, and machines.
2. Electronic devices: Materials like silicon, copper, and rare earth metals enable the production
of semiconductors, circuits, and electronic components.
3. Energy storage and conversion: Materials like lithium, nickel, and graphite are used in
batteries, solar panels, and fuel cells.
4. Transportation: Materials like steel, aluminum, and carbon fiber are used in vehicle
manufacturing, aerospace, and marine engineering.
5. Biomedical applications: Materials like titanium, stainless steel, and polymers are used in
medical implants, prosthetics, and drug delivery systems.
6. Thermal management: Materials like copper, silver, and graphite are used to manage heat in
electronics, engines, and buildings.
7. Optical applications: Materials like glass, plastics, and crystals are used in lenses, fibers, and
lasers.
8. Smart materials: Materials like shape-memory alloys, polymers, and hydrogels are used in
adaptive structures, sensors, and actuators.
9. Nanotechnology: Materials like nanoparticles, nanotubes, and graphene are used in catalysis,
energy storage, and electronics.
10. Sustainability: Materials like recycled plastics, bioplastics, and sustainable composites are
used to reduce environmental impact.

Materials science and engineering play a vital role in developing innovative materials and
technologies to address societal challenges and improve our quality of life.

Quality Control and Assurance in Engineering Contexts:

Quality control and assurance are essential in engineering contexts to ensure that products,
systems, and services meet specified requirements, standards, and regulations. Quality control
focuses on monitoring and controlling processes to prevent defects, while quality assurance
focuses on ensuring that quality control processes are in place and effective.

Quality Control:

1. Inspection and testing

2. Process monitoring and control
3. Defect identification and correction
4. Statistical process control

Quality Assurance:
1. Quality planning and policy
2. Quality management systems (ISO 9001)
3. Audits and assessments
4. Training and education
5. Continuous improvement

Benefits of Quality Control and Assurance:

1. Reliability and performance

2. Safety and risk reduction
3. Customer satisfaction
4. Reduced rework and waste
5. Cost savings
6. Compliance with regulations and standards
7. Improved reputation and brand image
8. Increased efficiency and productivity

Engineering Contexts:

1. Manufacturing (e.g., automotive, aerospace)

2. Construction (e.g., buildings, bridges)
3. Electronics and electrical engineering
4. Software development
5. Healthcare and medical devices
6. Energy and utilities (e.g., nuclear, renewable energy)
7. Transportation (e.g., automotive, aerospace, rail)

By implementing effective quality control and assurance processes, engineers can ensure that
their designs, products, and services meet the required standards, regulations, and customer
expectations, ultimately leading to improved performance, safety, and reliability.

Qualitative and Quantitative Analysis:

In chemistry, qualitative and quantitative analysis are used to identify and determine the amount
of substances present in a sample.

Qualitative Analysis:
Qualitative analysis in chemistry involves identifying the presence or absence of a particular
substance or functional group in a sample. It provides information about the chemical
composition of a sample without quantifying the amount of each component. Examples of
qualitative analysis in chemistry include:
- Chemical tests (e.g., flame test, precipitate test) to identify ions or functional groups
- Chromatography (e.g., TLC, HPLC) to separate and identify components
- Spectroscopy (e.g., IR, NMR) to determine molecular structure

Example: Using a flame test to determine the presence of metal ions in a sample. The color of
the flame indicates the presence of a particular metal ion (e.g., sodium produces a yellow
flame).

Quantitative Analysis:
Quantitative analysis in chemistry involves determining the amount or concentration of a
substance in a sample. It provides numerical information about the chemical composition of a
sample. Examples of quantitative analysis in chemistry include:

- Titration (e.g., acid-base, redox) to determine the amount of a substance

- Gravimetry (e.g., weighing a precipitate) to determine the amount of a substance
- Spectroscopy (e.g., UV-Vis, AAS) to determine the concentration of a substance

Example: Using acid-base titration to determine the concentration of acetic acid (CH3COOH) in
a sample. The volume of base required to neutralize the acid is used to calculate the
concentration of acetic acid.

In summary, qualitative analysis in chemistry identifies what substances are present, while
quantitative analysis determines how much of each substance is present.

Emerging Trends and Applications of Analytical Techniques for Engineering:

Here are some of the emerging trends and applications of analytical techniques for engineering
in chemistry ¹ ² ³:
- Miniaturization: The increasing portability of devices has revolutionized the field of analytical
chemistry, allowing for on-site testing and analysis.
- Green analytical chemistry: This branch of analytical chemistry focuses on sustainability and
minimizing the consumption of hazardous substances.
- Electrochemical analysis: This field is rapidly advancing due to technological advancements,
and is now being used in the development of sensors and biosensors.
- Nanoscale imaging and relations in zeolites: Techniques such as atom probe tomography and
confocal fluorescence microscopy are providing new insights into the properties and behavior of
zeolites.
- Operando spectroscopy: This technique is allowing researchers to study zeolites under
working conditions, providing valuable information on their performance and deactivation
mechanisms.

Instrumental Methods of Analysis:

Spectroscopy is a non-destructive instrumental method of chemical analysis that measures the
interaction between matter and electromagnetic radiation. The method involves:

1. Sample preparation: Preparing the sample for analysis, which may include dissolving it in a
solvent or grinding it into a powder.

2. Radiation source: Exposing the sample to a specific range of electromagnetic radiation, such
as visible light, ultraviolet (UV), infrared (IR), or nuclear magnetic resonance (NMR).

3. Interaction: The radiation interacts with the sample, causing the molecules to absorb or emit
energy at specific wavelengths.

4. Detection: Measuring the absorbed or emitted radiation using a detector, such as a

photomultiplier tube or a charge-coupled device (CCD).

5. Spectrum: Plotting the intensity of the radiation versus the wavelength or frequency, creating
a spectrum that represents the chemical makeup of the sample.

6. Analysis: Interpreting the spectrum to identify the chemical structure, bonding, and properties
of the sample.

Types of spectroscopy:

1. UV-Vis spectroscopy (absorption and emission)

2. IR spectroscopy (absorption)
3. NMR spectroscopy (absorption and emission)
4. Mass spectrometry (MS) (ionization and fragmentation)
5. Atomic absorption spectroscopy (AAS) (absorption)
6. Fluorescence spectroscopy (emission)

Spectroscopy is used to:

1. Identify and quantify chemical compounds

2. Determine chemical structure and bonding
3. Analyze the composition of mixtures
4. Study chemical reactions and kinetics
5. Detect and quantify trace amounts of substances

Spectroscopy has numerous applications in various fields, including:

1. Pharmaceutical analysis
2. Environmental monitoring
3. Food safety and quality control
4. Biomedical research
5. Materials science and engineering

In summary, spectroscopy is a powerful analytical technique that provides valuable information

about the chemical makeup of a sample by measuring its interaction with electromagnetic
radiation.

UV Spectroscopy:

Here's the information you requested about UV spectroscopy ¹:

Principle: Spectroscopy is the measurement and interpretation of electromagnetic radiation

absorbed or emitted when the molecules or atoms or ions of a sample move from one energy
state to another energy state. UV spectroscopy is a type of absorption spectroscopy in which
light of the ultra-violet region (200-400 nm) is absorbed by the molecule which results in the
excitation of the electrons from the ground state to a higher energy state.

Instrumentation:
1. Light Source: Tungsten filament lamps and Hydrogen-Deuterium lamps are the most widely
used and suitable light sources as they cover the whole UV region.
2. Monochromator: Most of the spectrophotometers are double beam spectrophotometers. The
radiation emitted from the primary source is dispersed with the help of rotating prisms.
3. Sample and reference cells: One of the two divided beams is passed through the sample
solution and the second beam is passed through the reference solution.
4. Detector: Generally, two photocells serve the purpose of the detector in UV spectroscopy.
5. Amplifier: The alternating current generated in the photocells is transferred to the amplifier.
The amplifier is coupled to a small servometer.
6. Recording devices: Most of the time amplifier is coupled to a pen recorder which is connected
to the computer.

Applications:
1. Detection of Impurities
2. Structure elucidation of organic compounds
3. Quantitative determination of compounds
4. Qualitative determination of compounds.

Various Types of Electronic Transitions:

You're referring to electronic transitions in molecular orbitals!

Sigma (σ) and pi (π) orbitals are types of molecular orbitals that describe the orientation of
electrons in a molecule.

Here are the types of electronic transitions you mentioned:

1. Sigma to sigma star (σ → σ*):
- An electron is promoted from a sigma bonding orbital to a sigma antibonding orbital.
- This transition typically requires high energy and is often associated with molecular
fragmentation.
2. Pi to pi star (π → π*):
- An electron is promoted from a pi bonding orbital to a pi antibonding orbital.
- This transition is often associated with molecular excitation and is important in
photochemical reactions.

Other types of electronic transitions include:

1. N → σ* (n → σ*):
- An electron is promoted from a non-bonding orbital (n) to a sigma antibonding orbital.
2. N → π* (n → π*):
- An electron is promoted from a non-bonding orbital (n) to a pi antibonding orbital.
3. σ → π* (sigma to pi star):
- An electron is promoted from a sigma bonding orbital to a pi antibonding orbital.
4. π → σ* (pi to sigma star):
- An electron is promoted from a pi bonding orbital to a sigma antibonding orbital.

These electronic transitions are important in understanding various molecular processes, such
as absorption spectroscopy, photochemistry, and molecular reactivity.

IR Spectroscopy:

Here's what I found on the principle, instrumentation and applications of infrared (IR)
spectroscopy ¹ ² ³:

Principle: IR spectroscopy is an analytical technique that takes advantage of the vibrational

transitions of a molecule. It involves the interaction of infrared light with a molecule, with a
wavelength range from 2,500 to 16,000 nm. The absorption of infrared radiation by a molecule
corresponds to the energy of its vibrational bonds.

Instrumentation: The main parts of an IR spectrometer are the radiation source, sample cells,
monochromators, detectors and recorder.

Here are the main parts of an IR spectrometer ¹ ²:

1. Radiation source: This should emit IR electromagnetic radiations which are steady, intense,
and extended over the desired wavelength.
2. Monochromator: This selects desired frequencies of IR radiations because the sample will
only absorb some specific frequencies of IR radiations.
3. Sample cells and sampling: IR spectroscopy is used for the characterization of different
samples like solid, liquid, and gas. The sampling of different phases should be done in a
material that is transparent to IR radiation.
4. Detector: This detects the transmitted IR radiation by the sample.
5. Recorder: This records the IR spectrum.

The radiation sources include Nernst glower, incandescent lamp, mercury arc, tungsten lamp,
globar source and nichrome wire. The sample cells are used for solid, liquid or gas samples.
Monochromators include prisms, gratings and filters. Detectors measure the intensity of
unabsorbed infrared radiation, and recorders record the IR spectrum.

Applications: IR spectroscopy has been of great significance to scientific researchers in many

fields such as protein characterization, nanoscale semiconductor analysis, space exploration,
analysis of gaseous, liquid or solid samples, identification of compounds, quantitative analysis,
information regarding functional groups of molecules and constitution of molecules, and to know
about interaction among molecules.

Chromatography:

Chromatography is a laboratory technique used to separate a mixture into its components ¹. The
mixture is dissolved in a fluid solvent (gas or liquid) called the mobile phase, which carries it
through a system on which a material called the stationary phase is fixed ² ¹. Chromatography is
based on the concept of partition coefficient, where any solute partitions between two immiscible
solvents ¹.

Here are some types of chromatography ¹:

- Affinity chromatography: This technique separates components of a mixture based on their

affinity towards the stationary phase of the system.
- Anion exchange chromatography: This technique separates negatively charged molecules by
their interaction with the positively charged stationary phase in the form of ion-exchange resin.
- Cation exchange chromatography: This technique separates positively charged molecules by
their interaction with negatively charged stationary phase in the form of ion-exchange resin.
- Column chromatography: This technique separates the components in a mixture based on
their differential adsorption with the stationary phase, resulting in them moving at different
speeds when passed through a column.
- Flash chromatography: This technique separates components of a mixture based on their
differential adsorption to the stationary phase.
- Gas chromatography: This technique separates molecules based on their retention time
depending on the affinity of the molecules to the stationary phase.
- Gel filtration chromatography: This technique separates molecules of different molecular sizes.
- High-performance liquid chromatography: This technique separates the components of a
mixture based on their affinity with the stationary phase.
- Hydrophobic interaction chromatography: This technique separates molecules on the basis of
their degree of hydrophobicity.

Gas Chromatography:
Gas-Liquid Chromatography (GLC) is a separation methodology that employs a gaseous mobile
phase, typically an inert gas like helium or a nonreactive gas like nitrogen, and a liquid
stationary phase ¹. GLC differs from other forms of chromatography in that the mobile phase is a
gas and the components are separated as vapors.

The principle of Gas-Liquid Chromatography (GLC) is based on the partitioning of the

components of a mixture between a gaseous mobile phase and a liquid stationary phase. The
separation occurs due to differences in the affinity of the components for the two phases.

Here's a step-by-step explanation of the principle:

1. Vaporization: The sample is vaporized and carried by the gaseous mobile phase into the
column.
2. Partitioning: The components of the sample partition between the gaseous mobile phase and
the liquid stationary phase.
3. Separation: The components separate based on their differences in affinity for the two
phases.
4. Migration: The separated components migrate through the column at different rates.
5. Detection: The components are detected as they exit the column.
6. Identification and quantification: The components are identified and quantified based on their
retention times and peak areas.

The GLC principle is based on the concept of partition coefficient, which is the ratio of the
concentration of a component in the stationary phase to its concentration in the mobile phase.

Gas-Liquid Chromatography (GLC) has a wide range of applications in various fields, including:

1. Analytical chemistry: GLC is used to analyze and identify the components of a mixture,
determine the purity of a substance, and detect trace amounts of impurities.

2. Pharmaceutical industry: GLC is used to analyze drugs, detect impurities, and determine the
potency of pharmaceutical products.

3. Forensic science: GLC is used in forensic analysis to identify and compare evidence, such as
drugs, explosives, and other substances.

4. Environmental monitoring: GLC is used to analyze air and water samples for pollutants, such
as pesticides, herbicides, and volatile organic compounds.

5. Food and beverage industry: GLC is used to analyze the composition of food and beverages,
detect adulteration, and determine the quality of products.
6. Petrochemical industry: GLC is used to analyze petroleum products, such as gasoline, diesel
fuel, and lubricating oils.

7. Biomedical research: GLC is used to analyze biological samples, such as blood, urine, and
tissue extracts, to diagnose diseases and monitor treatment.

8. Quality control: GLC is used in quality control to detect impurities, determine the purity of
substances, and monitor the production process.

High Performance Liquid Chromatography:

HPLC stands for high-performance liquid chromatography, an analytical technique used to

separate, identify and quantify each component in a mixture ¹ ². It is an advanced version of
column liquid chromatography and is used to identify and quantify the components of a mixture,
and has applications in pharmaceuticals, biotechnology, food and environmental analytics ¹.

The HPLC technique is based on the principle of column chromatography, where a mixture is
separated using a stationary and a mobile phase ². Here are the main steps involved in HPLC ¹
²:

1. Purification takes place in a separation column between a stationary and a mobile phase.
2. The stationary phase is a granular material with very small porous particles in a separation
column.
3. The mobile phase is a solvent or solvent mixture which is forced at high pressure through the
separation column.
4. The sample is injected into the mobile phase flow from the pump to the separation column
using a syringe.
5. The individual components of the sample migrate through the column at different rates
because they are retained to a varying degree by interactions with the stationary phase.
6. After leaving the column, the individual substances are detected by a suitable detector and
passed on as a signal to the HPLC software on the computer.
7. At the end of this operation/run, a chromatogram in the HPLC software on the computer is
obtained.
8. The chromatogram allows the identification and quantification of the different substances.

Here are some of the applications of HPLC chromatography ¹ ² ³ ⁴:

- Analysis of drugs and pharmaceuticals

- Medical diagnosis and research
- Detection of drugs and other substances for legal purposes
- Food and beverage safety
- Environmental monitoring
- Forensic and toxicology labs
- Quality control in manufacturing
- Proteomics and metabolomics research
- Biopharmaceuticals and biotechnology
- Academic and industrial research

Microscopy SEM:

Scanning Electron Microscope (SEM) is a type of electron microscope that produces images of
a sample by scanning the surface with a focused beam of electrons ¹ ². The electrons interact
with atoms in the sample, producing various signals that contain information about the surface
topography and composition of the sample. The electron beam is scanned in a raster scan
pattern, and the position of the beam is combined with the intensity of the detected signal to
produce an image.

The principle of Scanning Electron Microscopy (SEM) is based on the interaction between a
focused beam of electrons and the surface of a sample, producing various signals that contain
information about the sample's topography and composition.

The main principles are:

1. Electron Beam Formation: An electron gun produces a beam of electrons, which is focused
and condensed into a fine probe.
2. Beam Scanning: The focused beam is scanned across the sample in a raster pattern, similar
to a TV scan.
3. Electron-Sample Interactions: The beam interacts with the sample, producing various signals,
such as:
- Secondary Electrons (SE): emitted from the sample's surface, providing topographic
information.
- Backscattered Electrons (BSE): reflected from the sample's surface, providing information
on composition and atomic number.
- X-rays: emitted from the sample, providing elemental analysis.
4. Signal Detection: The signals are detected by specialized detectors, such as SE and BSE
detectors.
5. Image Formation: The detected signals are processed and combined to form a
high-resolution image of the sample's surface.

SEM's high resolution and depth of field allow for detailed imaging of the sample's surface
morphology, making it a powerful tool for materials science, biology, and nanotechnology
research.

Here's how SEM microscopy works ¹ ²:

1. An electron gun emits electrons, which are focused by the first condenser lens. The beam is
then narrowed by the condenser's aperture, filtering out high-angle electrons.
2. The fine probe current knob focuses the electrons via the second condenser lens into a
narrow, tightly focused, coherent beam.
3. An objective aperture removes high-angle electrons from the beam, which is then scanned by
a grid of coils.
4. The beam is focused on the desired area of the specimen by the objective lens, the final lens.
5. When the beam interacts with the sample, various devices detect the radiations produced.
These devices count the interactions before the beam advances to its next dwell point and
display a pixel on a CRT, the brightness of which is dependent on the number of interactions.
6. The scanning speed allows for 30 scans of the complete pattern in one second.

Scanning electron microscopy (SEM) is an important electron microscopy technique that is

capable of achieving a detailed visual image of a particle with high-quality and spatial resolution
¹. SEM is used in a variety of fields including ²:

- Industrial uses
- Nanoscience studies
- Biomedical studies
- Microbiology
- Spot chemical analysis in energy-Dispersive X-ray Spectroscopy
- Analysis of cosmetic components
- Study of the filament structures of microorganisms
- Study of the topography of elements used in industries.

Thermo Gravimetry TGA:

Thermogravimetric analysis (TGA) is a method of thermal analysis in which the mass of a

sample is measured over time as the temperature changes ¹. This technique provides
information about physical phenomena, such as phase transitions, absorption, adsorption and
desorption, as well as chemical phenomena including chemisorptions, thermal decomposition,
and solid-gas reactions. TGA is conducted on an instrument referred to as a thermogravimetric
analyzer, which continuously measures mass while the temperature of a sample is changed
over time.

The principle of Thermogravimetric Analysis (TGA) is based on the measurement of the change
in mass of a sample as it is heated or cooled in a controlled environment. The instrument
continuously monitors the sample's mass while the temperature is changed at a predetermined
rate.

Here's the step-by-step principle:

1. Sample preparation: A small sample (typically a few milligrams) is placed in a sample pan.

2. Heating/Cooling: The sample is then heated or cooled at a controlled rate (typically

1-100°C/min) in a furnace or oven.
3. Mass measurement: The sample's mass is continuously measured using a sensitive balance
or microbalance.

4. Data collection: The mass change vs. temperature data is collected and plotted as a
thermogram.

5. Analysis: The thermogram provides information about physical and chemical changes
occurring in the sample, such as:
- Mass loss or gain
- Phase transitions
- Decomposition
- Reaction kinetics
- Thermal stability

TGA provides valuable information about a material's thermal properties, helping researchers
understand its behavior under various temperature conditions.

Here are some applications of Thermogravimetric Analysis (TGA) ¹ ² ³:

- Analytical Chemistry: TGA is used in analytical investigations, such as studying the

decomposition of substances and materials.
- Inorganic Chemistry: TGA is used to distinguish between constitutional water and adsorbed
water, and to study the properties of inorganic compounds.
- Organic Chemistry: TGA is used to study the pyrolysis of organic materials, such as wood and
polymers.
- Materials Science: TGA is used to study the thermal properties of materials, such as
decomposition, oxidation, and combustion.
- Pharmaceuticals: TGA is used to study the thermal stability of pharmaceuticals and their
decomposition products.
- Food Science: TGA is used to study the thermal properties of food materials, such as moisture
content and thermal decomposition.
- Environmental Science: TGA is used to study the thermal properties of environmental
samples, such as soil and water.
- Petrochemical Industry: TGA is used to study the thermal properties of petrochemicals and
their decomposition products.
- Polymers Manufacturing: TGA is used to study the thermal properties of polymers and their
decomposition products.
- Plastic Manufacturing: TGA is used to study the thermal properties of plastics and their
decomposition products.
- Quality Control: TGA is used to study the thermal properties of materials and products, and to
ensure quality and safety.