Volume No.

Issue No.3

August 13, 2014

Infrared Spectroscopy: An Application

ABSTRACT
Spectroscopy is the study of absorption and emission of light and radiation. An application of this is infrared
spectrometer where it covers electromagnetic spectrum, specifically between visible to microwave region. IR
spectroscopy is helpful in identifying compound since no two structures can have the same IR spectra. Some of the
sampling handling techniques used in this experiment are pelleting, IR cells and ATR. This experiment aimed to
introduce infrared spectrometer as an analytical tool in description and possible identification of unknown material,
teach student the different sampling techniques for IR and to identify and interpret the important peaks in the IR
spectra. Solid, liquid and thin film samples were analysed using the different techniques stated earlier. It was found
out that the thin film sample contains ethylene or propylene as monomer. The liquid sample was found to be ethyl
chloroacetate. Lastly, the solid sample was identified to be Naphthalene.

INTRODUCTION
Spectroscopy is the study of absorption and emission
of light and radiation. This also includes the
interaction
between
particles.
Spectroscopic
techniques are based on measuring the amount of
radiation produced or absorbed by the substance.
Spectroscopic methods are classified depending on
the region of the electromagnetic spectrum such as
X-ray, ultraviolet (UV), visible, infrared (IR) and
microwave. This experiment focuses on Infrared
spectroscopy.
Infrared spectroscopy is a technique that covers the
region of electromagnetic spectrum from visible
(800nm) to short-wavelength microwave. The
infrared region has been divided into three groups:
near IR, mid-IR and far IR with range of decreasing
wavenumber. The spectrum produced primarily
depends on the vibrational motion between bonds of
the molecules. The energy levels absorbed by
infrared spectrometer are due to the vibrations of the
atoms, stretching and bending. Stretching vibration is
done when the atoms move back and forth with a
known separation distance called bond length.
Bending vibration is done when the bond axis of a
particular bond rock back and forth within or outside
the plane.

Wavenumbers are usually used to measure the

energy. These are usually expressed as cm -1. To
compute the wavenumber, these equations are used:

where is the wavelength, v is the frequency and c

is the speed of light at vacuum, 3x108 m/s.
During the absorption process, only bonds with
dipole moment that changes as function of time are
capable of absorption. Thus, symmetric compounds
do not absorb infrared radiation.
Infrared spectrum is used to identify molecular bonds
since it provides an excellent fingerprint of the
compounds. It can be used to identify different
functional groups such as carbonyls, carboxyls and
amine.
There are many sample handling techniques for IR
spectrometry. These are dependent on the properties
of the substance. Three of these techniques are using
cells, pelleting and ATR Spectra.
IR liquid cells are commonly used for highly
concentrated samples. There are many types of IR
window for this technique such as NaCl and KBr.
Since some of them are soluble to water, aqueous

Professor, School of Che-Chm, Mapa Institute of Technology

Student, CHM115L/A11, School of Che-Chm, Mapa Institute of Technology

2
solution couldnt be analysed. Pelleting uses KBr for
solid handling. In this technique, KBr is mixed to the
solid using mortar and pestle. This mixture is pressed
by transparent disk. ATR, attenuated total
reflectance, is used when less dense medium absorbs
evanescent radiation.

Figure 2. Mortar and Pestle

This studys purposes were to introduce infrared

spectrometer as an analytical tool in description and
possible identification of unknown material, teach
student the different sampling techniques for IR and
to identify and interpret the important peaks in the IR
spectra.

EXPERIMENTAL SECTION

Figure 3. ATR Accessory

The reagents used were KBr IR grade, Nojul, and

hexane. The unknown liquid and solid samples tested
were both sample number 7. The main instrument
used
was
the
Fourier
Transform-Infrared
Spectrometer. For the analyte preparation, the
material used was mortar and pestle.

Figure 4. FT-IR Spectrometer with Holder

.Figure 1. FT-IR Spectrometer

The thin film was analysed using ATR and direct

analysis. The film was cut into the desired
measurement patterned to the holder. The sample was
then analysed by FT-IR.
The solid sample was analysed using the ATR, and
KBr cell. Small amount of the sample was placed and
grinded in the mortar and pestle. When the solid was
already fine, 2 drops of nojul was added. The analyte
was mixed using the pestle. A drop was transferred to
the KBr cell and this was analysed by FT-IR.
The liquid sample was analysed using ATR and KBr
cell. For ATR, a drop of the sample was placed in the
sample holder and it was analysed by FT-IR. For KBr
cell, the syringe was filled with 2ml of the liquid

sample and was injected trough the KBr cell holder.

The liquid overflowed ensuring that enough volume
was placed inside the sample holder. After cleaning
the excess sample, the KBr sample cell holder was
placed inside FT-IR for analysis.

RESULTS AND DISCUSSION

For liquid sample observed in ATR, the spectra had a
strong broad band at 1736.53 cm-1 which signifies
that the compound is an ester. In 2982.32 cm-1, the
presence of C-H Stretch can be observed. At 781.10
cm-1, the presence of Cl was obvious. For liquid
sample observed in LC, the spectra observed in
2985.71 cm-1 is a C-H stretch. Lastly, in 782.24 cm-1,
the presence of Cl can be seen. Here, there are more
liquid sample spectra observed in ATR than the LC.
By the presence of molecular weight, the molecular
formula was obtained. It was found that the liquid
sample has a molecular formula of C4H7O2Cl. This is
ethyl chloroacetate which is an ester. Its structure is
shown in figure 5.

Figure 5. Structure of ethyl chloroacetate

Source: http://upload.wikimedia.org/wikipedia/commons/th umb/4
/49/Ethyl_chloroacetate.svg/512px-Ethyl_chloroacetate.svg.png

For thin film sample, the spectra had C-H stretch on

2858.29 cm-1 and 2929.49 cm-1. At 3072.74 cm-1, it
can be concluded as an alkene. At 2817.27 cm -1, sp2
can be observed. It can also be concluded that at
1720.99 cm-1, it is a ketone, and at 1426.53 cm-1, it is
an aromatic. The film was then identified to be
polyethylene like most of the plastics. Its chemical
formula is (C2H4)nH2. Its structure is shown in figure
6.

Figure 6. Structure of polyethylene

Source: http://upload.wikimedia.org/wikipedia/commons/f/f7/Pol
yethylene-repeat-2D-flat.png

For the solid sample, it was observed at 2853.78 cm-1,

that it has sp2-H. At 1606.21 cm-1 and 1692.06 cm-1, it
was concluded that it has C=C. At 841.14 cm -1,
917.88 cm-1, and 1011.27 cm-1, theres a presence of
O- . Lastly, at 2853.78 cm-1, aromatic ring can be
observed. With the presence of the molecular weight,
the molecular formula was obtained. It was found
that the solid sample has a molecular formula of
C10H8. This is naphthalene which is an aromatic. Its
structure is shown in figure 7.

Figure 7. Structure of naphthalene

Source:http://schoolworkhelper.net/wp-content/uplo ads/2011/06/
Naphthalene.png

CONCLUSION
The three objectives were achieved. Infrared
spectrometer was used in analysing unknown
compounds from the peaks that it had generated
which have corresponding interpretations on manuals
and books. Different sampling techniques such as
using KBr cell and ATR were applied for
identification of unknown samples. Lastly, the peaks
were identified properly using the appendices of
different references.
To enhance the experiment, it is recommended that
additional information about the sample must be

provided. Melting point and boiling point

determination can also be used as a basis for specific
analysis of the sample

REFERENCES
1. Pavia, D., et al., Introduction to Spectroscopy.

4th ed. 2009, Belmont: Brooks/Cole, Cengage

Learning. 657.
2. Skoog, D. A., Holler, F. J., West, D. M., and
Crouch, S. R. (2011) Fundamentals of Analytical
Chemistry, 8th Ed., Cengage Learning.
3. Skoog, D. A., Holler, F. J., and Crouch, S. R.
(2011) Principles of Instrumental Analysis, 6th Ed.,
Thomas Learning, Inc.
Websites:
1.

2.

3.

Chu, S. Infrared Spectroscopy. 2011 [cited;

Available from:
http://www.britannica.com/EBchecked/topic/558
901/spectroscopy/80625/Types-of-microwavespectrometer#ref620336.
Denisko, O. and A. Katritzky. Heterocyclic
compound. Ultraviolet, infrared, nuclear
magnetic resonance, and mass spectra [cited;
Available from:
http://www.britannica.com/EBchecked/topic/264
227/heterocyclic-compound/277865/Meltingand-boiling-points#ref1004803.
Noller, C., et al. Chemical compound. Infrared
spectroscopy 2011 [cited; Available from:
http://www.britannica.com/EBchecked/topic/108
614/chemical-compound/278329/Infrared-IRspectroscopy#ref615870.