HANDED IN BY:
CH ABDULLAH MAQSOOD 1937
Moorche
DR_ALEENA
PHAMACEUTICAL ANALYSIS
Infrared Spectroscopy:
(From Chatwal & Anand, Instrumental Methods of Chemical Analysis, 5th Ed.)
1. Definition
Infrared (IR) spectroscopy is an analytical method in which a molecule absorbs infrared
radiation and undergoes vibrational changes.
Each molecule absorbs IR light at specific wavelengths, producing a unique spectrum. This
spectrum works like a fingerprint for identification.
2. Principle
IR spectroscopy is based on the principle that:
Every chemical bond in a molecule vibrates (stretches or bends).
When IR radiation matches the natural frequency of these vibrations, the molecule
absorbs that radiation.
The amount of radiation absorbed at different wavelengths is recorded as peaks.
These absorption peaks help in recognizing functional groups such as –OH, –NH, C=O,
C–H, etc.
📘 Simple Explanation:
Like a tuning fork vibrates when hit by sound of the same frequency, a chemical bond vibrates
when it gets IR radiation of the same frequency.
3. Instrumentation of IR Spectrophotometer
A. IR Radiation Source
The source provides continuous IR radiation.
It must be stable, intense, and able to cover the whole IR region.
Common sources include:
Nernst Glower (heated oxide rod)
Globar (silicon carbide rod, gives strong IR)
Incandescent wire
B. Sample Handling System
Different sample forms need different techniques:
Solids:
o KBr pellet method: solid is mixed with dry KBr and pressed into a transparent
pellet.
o Nujol mull: solid dispersed in mineral oil.
Liquids:
o Placed between two salt plates (NaCl/KBr) because glass absorbs IR.
Gases:
o Gas cells with long path lengths are used.
C. Monochromator
Separates IR radiation into different wavelengths so that each wavelength can interact
individually with the sample.
Types:
Prism
Diffraction grating
D. Detector
The detector senses the IR radiation that has passed through the sample and converts it into an
electrical signal.
Common detectors:
Thermocouple detector – generates voltage on heating
Golay cell – sensitive to gas expansion
Pyroelectric detector – fast and widely used
E. Readout / Recorder / Computer System
The electrical signal from the detector is amplified and converted into a readable IR spectrum.
Modern instruments use digital displays and computer software.
Block Diagram
IR Source → Sample → Monochromator → Detector → Amplifier → Recorder/Display
4. Applications
Identification of Functional Groups: IR gives clear peaks for OH, NH, C=O, etc.,
helping identify structure.
Purity and impurity check: Impurities cause extra or shifted peaks.
Structural elucidation: Helps confirm presence/absence of specific bonds.
Drug–excipient compatibility: Used in formulation studies.
Quality control in pharmaceutical industries: Fast and reliable technique.
FTIR (Fourier Transform Infrared
Spectroscopy)
(From Chatwal & Anand, Instrumental Methods of Chemical Analysis, 5th Ed.)
1. Definition
FTIR is a modern form of infrared spectroscopy where all IR frequencies are scanned
simultaneously, and a Fourier Transform is applied to convert the raw signal (interferogram)
into a readable IR spectrum.
2. Principle
FTIR operates on two combined principles:
A. IR Absorption Principle
The sample absorbs IR radiation at frequencies matching the vibrational energy of its chemical
bonds.
This forms an IR absorption spectrum unique to the compound.
B. Fourier Transform Principle
FTIR uses a device called a Michelson Interferometer.
Instead of scanning one wavelength at a time, it collects all wavelengths at once.
The output is an interferogram (complex signal).
A mathematical process called Fourier Transform converts it into a normal IR
spectrum.
📘 Easy Explanation:
FTIR is faster and more accurate because it takes the whole IR data in one shot, rather than
slowly scanning wavelength by wavelength.
3. Instrumentation of FTIR
FTIR spectrometer mainly includes:
A. IR Source
Same sources as conventional IR:
Globar
Nernst glower
Incandescent wire
Provides a continuous IR beam.
B. Michelson Interferometer (Heart of FTIR)
This is the key component that makes FTIR different.
It contains:
Beam splitter
Fixed mirror
Moving mirror
Function:
Splits IR beam into two paths
Recombines them to create an interference pattern (interferogram)
This contains information of all IR frequencies at once
C. Sample compartment
The interferogram passes through the sample, and absorption occurs according to molecular
vibrations.
Sample forms:
Solid (KBr pellet)
Liquid (NaCl plates)
Gas (gas cells)
D. Detector
Highly sensitive detectors are used because FTIR collects many frequencies:
Pyroelectric detector
Golay cell
Thermocouple detector
E. Computer System
The detector output is processed using Fourier Transform to convert interferogram → IR
spectrum.
The final spectrum appears on the screen with peaks showing functional groups.
4. Advantages of FTIR
Faster (collects all wavelengths at once)
Higher resolution and accuracy
Better signal-to-noise ratio
No mechanical scanning required
Highly reliable and reproducible results
5. Applications
Identification of unknown compounds
Detection of functional groups
Drug purity testing
Studying drug–excipient interactions
Quantitative analysis of pharmaceuticals
Polymer and packaging material analysis
BASIC DEFINATIONS:
1. Frequency (ν)
According to Pavia, frequency is the number of complete wave cycles that pass a point in one
second.
Measured in Hz (s⁻¹).
Frequency is directly related to the energy of the radiation.
➡️Source: Pavia – Introduction to Spectroscopy, IR Chapter (relationship of frequency with
energy)
2. Wavelength (λ)
wavelength as the distance between two consecutive peaks or troughs of a wave.
In IR spectroscopy, wavelength may be given in micrometers (µm).
Wavelength and frequency are inversely related:
ν=c/λ
➡️Source: Pavia – Introduction to Spectroscopy, Basic Wave Properties
3. Wave Number (ṽ)
wavenumber as the number of waves per centimeter.
It is measured in cm⁻¹.
Wavenumber is commonly used in IR spectra because it is directly proportional to
frequency and energy.
➡️Source: Pavia – Introduction to Spectroscopy, IR Units (cm⁻¹)
4. Functional Group Region (IR)
Pavia divides the IR spectrum into regions.
The functional group region is from 4000–1500 cm⁻¹.
It contains strong and sharp absorptions due to major functional groups.
Examples: O–H, N–H, C=O, C≡N, C≡C.
➡️Source: Pavia – IR Spectroscopy Chapter, Functional Group Region
5. Fingerprint Region (IR)
The fingerprint region as the area from 1500–400 cm⁻¹.
It contains complex absorption patterns unique to each compound.
Very useful for confirming identity of a molecule.
➡️Source: Pavia – IR Spectroscopy Chapter, Fingerprint Region