Presentation
on
IR Spectroscopy
Md. Tayfuzzaman, Executive-MD&V
Key Points to Discuss
Definition of IR Interferometer
Spectrophotometry Absorption bands
Basic theory ATR
Vibrational modes Sample preparation
Instrumentation Application
FTIR
Difference of FTIR and
IR
Definition of IR Spectroscopy
IR spectroscopy is the spectroscopy that deals with the infrared
region of the electromagnetic spectrum, that is light with a
longer wavelength and lower frequency than visible light. Its
and absorption spectroscopy.
Typical units of frequency used in IR spectra are reciprocal
centimeter (cm-1)
The infrared portion of the electromagnetic spectrum divide
into three region—
1. Near infrared (NIR) 14000 to 4000 cm-1 (800 to 2500 nm)
2. Mid infrared 4000 to 400 cm-1 (2.5 to 25 um)
3. Far infrared 400 to 10 cm-1 (25 to 1000 um)
Basic theory
In the IR spectroscopic technique the molecule of interest
absorb specific frequencies of electromagnetic radiation. This
absorb frequencies are directly depends on their molecular
structure. The absorb frequencies and the transmitted
vibrational energies from the specific bond or functional
groups make resonance.
The intensity of resonance frequency depends on the
following matters
Molecular ground state electronic potential
Bond strength
Mass of the either end of the bond
Vibrational mode
Vibrational mode
An IR active molecule should have vibrational modes, which is
created by the change in dipole moment.
A molecule can vibrate in many ways and each way is called
vibrational band.
If a linear molecule have n numbers of atoms it will have 3n-
5 vibrational modes or degrees of vibrational modes, where
as for the non leaner molecules it will be 3n-6.
Simple diatomic and symmetrical molecules doesn’t have the
sufficient vibrational band to be an IR active.
On the other hand asymmetrical and complex molecule have
many bonds and consiquently many vibrational degree of
freedom. This will result number of peaks in their IR spectra.
Example of Different Vibrational
Modes
Instrumentation
A source generate light across the spectrum of interest.
A monochromator separates the source radiation into its
different wavelength.
A slit allow required light to pass through the sample.
Sample absorbs light according to their chemical properties.
A detector collect the radiation that passes through the
sample.
Unlike the UV spectrophotometer it may also facilitate with
double beam system to collect and compare the spectra of
reference and test sample.
Schematic Diagram of IR
FTIR (Fourier Transform Infrared
spectrophotometry)
In this technique light is guided through an interferometer and
than through the sample. A moving mirror inside the
apparatus alters the distribution of infrared light that passes
through the interferometer. The signal directly recorded
called an interferogram represent the light output as mirror
position.
A data processing technique called as Fourier transform convert
this raw data as a desired sample spectrum.
Difference between Dispersive IR and
FTIR
Dispersive IR spectrophotometry take
absorption of one monochromatic IR light at
a time and sum those up to draw the
spectrum.
On the other hand in a FTIR, its capable to take
absorption of multi-chromatic light at a time.
For data collection it use Fourier transform.
This technique is more faster and effective
than the dispersive IR.
Schematic Diagram of FTIR
Interferometer
In a Michelson interferometer adapted for
FTIR, light from the polychromatic infrared
source, approximately a black-body radiator,
is collimated and directed to a beam splitter.
Ideally 50% of the light is refracted towards the
fixed mirror and 50% is transmitted towards
the moving mirror. Light is reflected from the
two mirrors back to the beam splitter and
(ideally) 50% of the original light passes into
the sample compartment. There, the light is
focused on the sample.
Schematic Diagram of Interferometer
Absorption Bands
Attenuated Total Reflections
With ATR sampling we direct the IR beam into a
crystal of relatively higher refractive index. The IR
beam reflects from the internal surface of the crystal
and creates an evanescent wave which projects
orthogonally into the sample in intimate contact
with the ATR crystal. Some of the energy of the
evanescent wave is absorbed by the sample and the
reflected radiation (some now absorbed by the
sample) is returned to the detector. (USP 197A)
In this technique sample refractive index should less
than that of ATR crystals.
Schematic Diagram of ATR
Sample Preparation
For the ATR there is no need prepare sample.
For the other techniques and gaseous sample we need sample
preparation.
Solid samples can be prepared for the IR examination by several
other methods.
1. A mull is prepared by grinding the sample with mineral oil and
sandwiching the resulting paste between sodium chloride plates.
2. The solid can be dissolved in a solvent and placed in a special
cell, called a solution cell, which is made of Sodium chloride.
This gives what is called solution spectrum.
3. A KBr pellet is prepared by grinding the solid sample with solid
Potassium brommide and applying great pressure to the dry
mixture. Potassium bromide is chosen because it is transparent
to infrared radiation. (USP 197K)
Liquid Sample Preparation
To prepare a liquid sample to IR analysis, firstly place a drop
of the liquid on the face of a highly polished salt plate (such
as NaCl, AgCl or KBr), then place a second plate on top of the
first plate so as to spread the liquid in a thin layer between
the plates, and clamps the plates together. Finally wipe off
the liquid out of the edge of plate. You can mount the
sandwich plate onto the sample holder. After finishing your
experiment, clean the plates with isopropanol (No water!) and
return them to the desiccators.
Precaution: Volatile liquid can’t be prepared with this method,
because it will evaporate while its spectrum is being obtained.
If the liquid sample is toxic or smelly, please don’t use this
method. In addition, NaCl and KBr are dissolved into water,
and thus they can’t be used for aqueous samples.
Compact Liquid cell
Demountable path length cell is designed for volatile liquid
sample. Assemble the cell as shown in the drawing. Then use
a syringe to fill the liquid into the cell. Finally seal the cell.
Liquid Cell
Gaseous Sample Preparation
Gas samples are generally measured by the transmission
method using a gas cell.
Each end is covered with a KBr or KRS-5 window that
transmits infrared light.
As the infrared light passes through the gas cell only
once, the gas cell internal pressure is slightly increased
when measuring low-concentration samples.
To introduce a gas sample into these gas cells, first
connect one of the taps to a vacuum pump and open it
to evacuate the cell. After closing the tap, connect the
other tap to the sample and open it to fill the gas cell
with the gas sample. Set the internal pressure from
several tens of Torr to 760 Torr.
Gas Cell
Application of IR Spectroscopy
1. Identification of raw materials
2. Identification of suspected counterfeit
samples.
3. Identification of extraneous matter.
4. Confirmation of chemical structure.
5. Identification of API in drug products.
Thank You
