UNIVERSITI TEKNOLOGI MARA SHAH ALAM

FACULTY OF APPLIED SCIENCES

BACHELOR OF ENVIRONMENTAL TECHNOLOGY

CHM 571 - BASIC INSTRUMENTAL ANALYSIS

LAB REPORT EXPERIMENT FOURIER TRANSFORM INFRARED

(FTIR) SPECTROSCOPY

NAME: MUHAMMAD WAZIF BIN MAZLAN

GROUP: AS229 2A

ID: 2018435614

LECTURER NAME: MADAM NORAINI KASIM

Abstract:

In this experiment, we carried out an experiment which involves Fourier Transform Infrared
(FTIR) Spectroscopy. IR is used to gather information about compound's structure, assess its
purity, and sometimes to identify it. Infrared radiation is that part of the electromagnetic
spectrum between the visible and microwave regions. Infrared radiation is absorbed by
organic molecules and converted into energy of molecular vibration, either stretching or
bending. Different types of bonds, and thus different functional groups, absorb infrared
radiation of different wavelengths. An IR spectrum is a plot of wavenumber (X-axis) vs
percent transmittance (Y-axis). Provided with the materials which consist of (paraffin oil,
acetophenone and toluene) liquid form and caffeine (solid form), these samples will undergo
spectroscopy using the FTIR machine which is called Perkin Elmer Spectrum One FTIR,
which is manually conducted by using a computer interconnected to the FTIR machine. The
machine will “scan” show the stretching and bending frequency bands of the functional
groups where the result from the machine will be printed out.

Depending on which functional group does the IR absorption belongs to, it will show
different types of wavenumbers depending on which stretching and bending frequency bands
they are categorized at the table. The purposes this experiment were conducted to recognizing
the characteristic stretching and bending frequency bands of the functional groups and to
identify the structure of an unknown sample.

Hypothesis:
By comparing the IR spectra of the pure compound using the tables of functional groups
frequencies and the spectra, the structure of unknown sample can be discovered.
Procedure:

A. Liquid sample

Two salt plates were rinsed using chloroform and wiped dry. A sample of liquid Paraffin was
taken and one drop of liquid Paraffin was added onto one of the salt plates. The liquid was
squeezed between two salt plates to give a layer that has a thickness of 0.01mm or less. The
two plates, held together by capillary action were then mounted in the beam path of the
spectrophotometer. The results were printed as a graph. The steps above were repeated for
another two more samples which are acetophenone and toluene.

B. Potassium bromide, KBr pellets for solid sample

Approximately 1mg of Caffeine solid sample was ground until they form fine powder. A few
milligrams of KBr were added and the mixture was ground again where the ratio needs to be
in the form of 1:9. To make the KBr pellet, the die pin from the storage container, as shown
in figure 1, was removed. The collar was placed on the lower anvil. Powdered KBr was then
placed in the collar until all the surface of the lower anvil was covered evenly. After that, the
upper anvil was placed so that it came into contact with the sample. The hand press was held
in upright position. The handle was lifted and the pressure dial at the top of the press was
rotated counter clockwise one revolution from full clockwise position. The die set was then
carefully placed in the hand press. To close the handle, the pressure dial was rotated
clockwise until the upper ram of the hand press touched the upper anvil of the die assembly.
The handle was opened and the dial was rotated clockwise three to five times. After about 20
seconds, open the KBr hand press and the pellet infrared spectrum were measured.
Afterwards, the pellet was removed from the collar and the entire die set was stored back into
the desiccator.
Result:

1. Polystyrene

Functional Group Molecular motion Wavenumber (cm-1)

Aromatics C-H stretch 3001.58

Alkane C-H stretch 2850.07

Aromatics C-H bend 756.99

Aromatics C-H bend 700.75

2. Caffeine
Functional group Molecular motion Wavenumber (cm-1)

Alkenes C=C stretch (isolated) 1698.40

Amides C=O stretch 1659.37

N-H stretch 3113.32

Amine C- N stretch (alkyl) 1239.37

3. Paraffin oil

Functional group Molecular motion Wavenumber (cm-1)

Alkane C-H stretch 2924.64

CH2 bend (4 or more) 722.02

CH3 bend 1377.60

4. Acetophenone

Functional group Molecular motion Wavenumber (cm-1)

Ketone C=O stretch 1683.00

C-C stretch 1266.17

Alkane CH3 bend 1359.91

 C- H bend (ortho) 760.10
Aromatic C=C stretch 1599.23

C-H stretch 3063.39

5. Toluene

Functional group Molecular motion Wavenumber (cm-1)

C-H stretch 3027.35

Aromatic
C=C stretch 1604.52
C-H bend 728.61

Alkane C-H stretch 2921.54

6. Unknown A

Functional Group Molecular motion Wavenumber (cm-1)

Alkanes C-H stretch 2837.32

Alcohols C-O stretch 1292.56

 Alcohols C-O stretch 1072.91

Discussion:

Before performing the experiment, a background check was done on the FTIR machine to
ensure that the machine is in a good condition by running a blank spectrum. The machine was
calibrated using a standard polystyrene film which the calibrated marks are given. Many
advantages that obtained using this device such as high sensitivity, high resolution and speed
of data acquisition. When a molecule absorbs infrared radiation, those frequencies of IR
radiation will match the natural vibrational frequencies of the molecule are absorbed and will
increase the amplitude of the vibrational motions of the bonds in the molecules. By
comparing the IR spectra, it is observed that the machine was properly calibrated and it is in
its tip top condition. Fourier Transform Infrared (FTIR) devices helped to overcome the
limitation encountered with the dispersive instrument. In this experiment, sampling handling
technique will have covered for liquid and solids. In this experiment, polystyrene, paraffin
oil, acetophenone and toluene were prepared as liquid sample. While caffeine was prepared
as solid sample (mull). Based on the result, many functional group identified each of the
sample such alkane, alkene, aromatics, alcohol and etc. For the unknown sample A, the
functional group that present were alkane and alcohol. So, this sample generally an alcohol
compound.

Conclusion:

This conclusion is purely based on the observation and the data from the stretching frequency
bands in the graph, where the absorbed wavenumbers showed the presence of alcohol and
alkane functional groups. The qualitative analysis of the IR spectra of some liquid samples
were carried out and the structure of the unknown sample A is alcohol.

Reference:

1. <IR Absorptions Table for Representative Functional Groups>

http://www.instruction.greenriver.edu/kmarr/chem
 %20162/Chem162%20Labs/Interpreting%20IR%20Spectra/IR%20Absorptions
%20for%20Functional%20Groups.htm

2. D. L. Pavia, G. M. Lampman, G. S. Kriz, J. R Vyvyan (2001). Introduction to

Spectroscopy, Fourth Edition. USA; Department of Chemistry Western Washington.