Instrumentation and applications of IR Spectroscopy

Instrumentation of IR

COMPONENTS:

1. Radiation source

2. Monochromator

3. Sample cell

4. Detector

5. Recorder

Radiation sources:

The main sources of IR radiation –

• Nichrome wire,
• Nernst Glower, which is a filament containing oxides of Zr, Th, Ce held together with a
binder. When they are electrically heated at 1200 – 2000 0C they glow and produce IR
radiation.

Monochromator:

It allows light of required wavelength to pass through, but absorbs the light of other wavelength.

Sample cell:

The cell holding the test sample must be transparent to IR radiation.

Detector:

IR detectors generally convert thermal radiant energy into electrical energy. The following are
important among the many. Photo conductivity cell, thermocouple, pyroelectric detectors.

Recorder:

The recorder records the signal coming out of the detector.

Working of IR Spectrophotometer:

The radiation emitted by the source is split into two identical beams having equal intensity. One
of the beams passes through the sample and the other through the reference sample. When the
sample cell contains the sample, the half beam traveling through it becomes less intense.

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Unit V – Annexure Dr. V.L.Nirmal Bhargavi
When the two half beams (one coming from the reference and the other from the sample)
recombine and produce an oscillating signal, which is measured by the detector. The signal from
the detector id passed to the recording unit and recorded.

Applications of IR Spectroscopy:

1. Identity of the compound:

The IR spectrum of the compound is compared with that of known compounds.
From the resemblance of the two spectra, the nature of the compound can be established.
This is because a particular group of atoms gives a characteristic absorption band in the
IR Spectrum.

Example: IR Spectra of both benzaldehyde and phenyl methyl ketone show a sharp
absorption peak at 1700 cm-1. This indicated the presence of C=O group in both the
compounds.

2. Detection of Functional groups:

In a given environment, a certain functional group will absorb IR energy of very nearly
the same wavelength in all molecules.
Examples:
Acetone CH3 – CO – CH3 and Diethyl ketone C2H5-CO-C2H5 give absorption peak at
the same place.
Acetic acid CH3COOH and Cyclobutanone CH2 – CH2 give absorption peak at
different places.
C=O
CH2 – CH2
3. Testing purity of a sample:
Pure sample will give a sharp and well resolved absorption bands. But impure sample
will give a broad and poorly resolved absorption bands. Thus by comparison with IR
spectra of pure compound, presence of impurity can be detected.
4. Study of progress of a chemical reaction:
The progress of a chemical reaction can be easily followed by examining the IR spectrum
of test solution at different time intervals.
5. Determination of shape or symmetry of a molecule
IR spectrum of NO2 gives 3 peaks at 750, 1323 and 1616 cm-1. S ince the spectra shows
only 3 peaks, it is confirmed that NO2 molecule is a non linear (bend) molecule.
6. To study Tautomerism:
Tautomeric equilibria can be studied with the help of IR spectroscopy.
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Unit V – Annexure Dr. V.L.Nirmal Bhargavi
 7. Industrial applications:
Determination of structure of chemical products
Determination of molecular weight
Crystallinity
8. Isomers can be identified in the finger print region.
Similar molecules may show very similar spectra in the group frequency region (4000 –
1430 cm-1). But, they show some differences in the finger print region (1400 – 700 cm-1)

The IR spectrum of the above three isomers in the group frequency region are almost
similar. But these are identified from their IR spectra in the fingerprint region, due to three
different absorptions.

9. Determination of Hydrogen bonding in a molecule

To detect the hydrogen bond and also distinguish between inter and intra molecular
hydrogen bonding present in a compound, a series of IR spectra of the compound at
different dilutions are taken. The solution of an alcohol at high concentrations gives two
peaks.
i) One sharp peak at 3630 cm-1 due to free -OH group.
ii) Another broad peak at 3500 – 3200 cm-1 due to –H bonded –OH group.

On dilution it is observed that the peak at 3630 cm-1 becomes more intense as the
concentration of the free –OH group increases. At the same time broader peak at 3500 –
3200 cm-1 becomes less intense and disappears at larger dilutions.

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Unit V – Annexure Dr. V.L.Nirmal Bhargavi
 The above explanation is applicable to –OH groups involved in intermoleculat H-
bonding. If the –OH group is involved in intra molecular hydrogen bonding, dilution will
not affect the intensity of the peak.

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Unit V – Annexure Dr. V.L.Nirmal Bhargavi