Infrared Spectroscopy

‫رقيه عماد جمال حسنين‬:‫االسم‬

‫الكمياء التطبيقيه‬:‫الشعبة‬
20211133:‫الكود‬

DECEMBER 5, 2023
APPLIED CHEMISTRY
HELWAN UNIVERSITY
 Contents:
-Basic Principles
-Instrumentation
-Sampling Technique
-Applications
What is IR Spectroscopy?
Infrared spectroscopy (IR spectroscopy)deals with the infrared
region of the electromagnetic spectrum, i.e. light having a longer
wavelength and a lower frequency than visible light. Infrared
Spectroscopy generally refers to the analysis of the interaction of a
molecule with infrared light.
The IR spectroscopy concept can generally be analyzed in three
ways: by measuring reflection, emission, and absorption. The
major use of infrared spectroscopy is to determine the functional
groups of molecules, relevant to both organic and inorganic
chemistry.
IR Spectroscopy detects frequencies of infrared light that are
absorbed by a molecule. Molecules tend to absorb these specific
frequencies of light since they correspond to the frequency of the
vibration of bonds in the molecule.

Regions of the Infrared spectrum

Most of the bands that indicate what functional group is present
are found in the region from 4000 cm-1 to 1300 cm-1. Their bands
can be identified and used to determine the functional group of an
unknown compound.
Bands that are unique to each molecule, similar to a fingerprint, are
found in the fingerprint region, from 1300 cm-1 to 400 cm These
bands are only used to compare the spectra of one compound to
another.

Theory of IR-spectroscopy:
IR Spectroscopy measures the vibrations of atoms, and based on this
it is possible to determine the functional groups. Generally, stronger
bonds and light atoms will vibrate at a high stretching frequency
(wavenumber).

In order for a vibrational mode in a molecule to be "IR

Active ", it must be associated with changes in the permanent
dipole. A molecule can vibrate in many ways, and each way is called
a vibrational mode.

Linear molecules have 3N - 5 degrees of vibrational modes whereas

nonlinear molecules have 3N - 6 degrees of vibrational modes (also
called vibrational degrees of freedom. As an example H2O, a non-
linear molecule, will have 3 × 3 - 6 = 3 degrees of vibrational
freedom, or modes.

Molecular vibrations to Infrared radiations

There are six types of vibration usually encountered in IR spectroscopy:

(1) Asymmetrical stretching

(2) Symmetrical stretching
(3) Bending and scissoring
(4) Rocking or in-plane bending
(5) Twisting
(6) Wagging

IR Spectroscopy Instrumentation
The main parts of the IR spectrometer are as follows:
1. Radiation source
IR instruments require a source of radiant energy which emits IR
radiation which must be steady, intense enough for detection, and
extend over the desired wave length .Various radiation sources are
known, such as Nernst glower, Mercury arc, Tungsten lamp, etc.
2. Sample cells and sampling of substances
IR spectroscopy has been used for the characterization of solid,
liquid, or gas samples.
1- Solid – Various techniques are used for preparing solid samples
such as pressed pellet technique, solid run in solution, solid films,
mull technique, etc.
2-Liquid – Samples can be held using a liquid sample cell made of
alkali halides. Aqueous solvents cannot be used as they will dissolve
alkali halides. Only organic solvents like chloroform can be used.
3- Gas– Sampling of gas is similar to the sampling of liquids.
3. Monochromators
Various types of monochromators are can be used, such as prism,
gratings and filters.
4. Detectors
Detectors are used to measure the intensity of unabsorbed infrared
radiation. Detectors like thermocouples, Bolometers, thermistors,
Golay cell, and pyro-electric detectors are used.
5. Recorder
Recorders are used to record the IR spectrum.
IR Chart or spectrum
An IR spectrum is essentially a graph plotted with the infrared light
absorbed on the Y-axis against frequency or wavelength on the X-
axis. Given below is a sample of typical IR spectrum.

Sampling Technique
IR spectroscopy is used for the characterization of solid, liquid or
gas samples. Material containing sample must be transparent to the
IR radiation. So, the salts like NaCl , KBr are only used.
1. Sampling of solids
Various techniques used for preparing solid samples are as follows
a) Mull technique: In this technique, the finely crushed sample is
mixed with Nujol (mulling agent) in n a marble or agate mortar,
with a pestle to make a thick paste. A thin film is applied onto the
salt plates. This is then mounted in a path of IR beam and the
spectrum is recorded.
b) Solid run in Solution – In this technique, solid sample may be
dissolved in a non-aqueous solvent provided that there is no
chemical interaction with the solvent and the solvent is not
absorbed in the range to be studied. A drop of solution is placed on
the surface of alkali metal disc and solvent is evaporated to dryness
leaving a thin film of the solute.
c) Case film technique – If the solid is amorphous in nature then the
sample is deposited on the surface of a KBr or NaCl cell by
evaporation of a solution of the solid and ensured that the film is
not too thick to pass the radiation.
d) Pressed pellet technique – In this technique, a small amount of
finely ground solid sample is mixed with 100 times its weight of
potassium bromide and compressed into a thin transparent pellet
using a hydraulic press. These pellets are transparent to IR radiation
and it is used for analysis.
2. Sampling of liquids
Liquid sample cells can be sandwiched using liquid sample cells of
highly purified alkali halides, normally NaCl. Other salts such as KBr
and CaF2 can also be used. Aqueous solvents cannot be used
because they cannot dissolve alkali halides. Organic solvents like
chloroform can be used. The sample thickness should be selected so
that the transmittance lies between 15-20%. For most liquids, the
sample cell thickness is 0.01-0.05 mm. Some salt plates are highly
soluble in water, so the sample and washing reagents must
be anhydrous
3. Sampling of gases
The sample cell is made up of NaCl, KBr etc. and it is similar to the
liquid sample cell. A sample cell with a long path length (5 – 10 cm)
is needed because the gases show relatively weak absorbance.

Applications of IR Spectroscopy
IR spectroscopy is a widely used analytical technique in a
variety of fields, including chemistry, materials science,
and biochemistry. Moreover, it is applied as follows:
Identification of an organic
Compound : Functional groups, for example, two compounds with
similar overlay able spectra must have the same functional groups.
Interestingly, an FT-IR spectrophotometer is used at airports to
detect drug addicts.

Purity of chemical compound: Although thorough FTIR is not

commonly used as a quantitative analysis, it is useful for
determining the purity of chemical compounds.

Reaction progress: Organic chemical reactions are slow, so their

progress is to be measured after timeintervals through IR
spectroscopy of the mixture.

References:
-https://www.pharmatutor.org
-https://byjus.com