FACULTY OF APPLIED SCIENCES

CHM 571 - BASIC INSTRUMENTAL ANALYSIS

LAB REPORT

NAME: MOHAMAD SAIFUL BIN MOHD RAFFIAH

STUDENT ID: 2021459156
CLASS GROUP: AS239 4A
EXPERIMENT 4: FOURIER TRANSFORM INFRARED (FTIR)
SPECTROSCOPY
LECTURER: DR. NORAINI BINTI KASIM
DATE OF EXPERIMENT: 17th MAY 2023
DATE OF SUBMISSION: 2nd JULY 2023
Tittle : Fourier Transform Infrared (FTIR) Spectroscopy

Objective
1. To carry out qualitative analysis of the IR spectra of some liquid samples by identifying the
characteristics stretching and bending frequency bands of the functional group.
2. To identify the structure of an unknown sample by identifying the characteristics functional
group frequencies of the IR spectra and the molecular formula. Confirmation of the structural
formula can be made by comparing the IR spectra of the pure compounds.

Introduction
The most popular type of infrared spectroscopy is FTIR. All infrared spectroscopies work on the
idea that some infrared (IR) radiation is absorbed when it passes through a sample. The radiation
emitted by the sample is measured. Because various molecules emit different spectra due to their
different structures, the spectra can be utilised to identify and discriminate between molecules. In
this sense, the spectra are almost identical to people's fingerprints or DNA. Organic synthesis,
polymer science, petrochemical engineering, pharmaceutical industries, and food analysis all use
FTIR spectroscopy. In other words, it can be used for everything from monitoring processes to
identifying substances to determining the components of a mixture.

Covalent bonds in a molecule selectively absorb radiation of specific wavelengths, causing the
vibrational energy of the bond to vary. The type of vibration caused by infrared radiation
(stretching or bending) is determined by the atoms in the bond. Because different bonds and
functional groups absorb different frequencies, the transmittance pattern for each molecule is
unique (the inverse of absorbance is transmittance). The spectrum is plotted on a graph, with the
X-axis representing wavenumber (cm-1) and the Y-axis representing transmittance (wavenumber
is 1/wavelength and correlates to the energy of molecular bond vibration).

Procedures
A. Liquid sample
1. Two salt plates were rinsed and dried with chloroform. A drop of liquid Paraffin was applied
to one of the salt plates after a sample of liquid Paraffin was taken.
2. The liquid was compressed between two salt plates to create a layer with a thickness of
less than 0.01mm. The two plates, held together by capillary action, were then placed in
the spectrophotometer's beam path.
3. The results were graphed and printed. The above methods were repeated for two
additional samples, acetophenone and toluene.
B. Potassium bromide, KBr pellets for solid sample
1. 1 mg of Caffeine solid sample was crush into a fine powder. A few mg of KBr were added,
and the mixture was processed again to the required ratio of 1:9.
2. To create the KBr pellet, the die pin from the storage container was removed, as illustrated
in Figure 1.
3. The collar was secured to the bottom anvil. The collar was then filled with powdered KBr
until the entire surface of the lower anvil was equally covered. The higher anvil was then
positioned so that it made contact with the sample. The upright position of the hand press
was maintained.
4. Lifting the handle, the pressure dial at the top of the press was rotated anticlockwise one
revolution from the full clockwise position. After that, the die set was carefully placed in the
hand press. To close the handle, turn the pressure dial clockwise until the upper ram of the
hand press made contact with the upper anvil of the die assembly.
5. The handle was pulled open, and the dial was rotated three to five times clockwise. After
roughly 20 seconds, open the KBr hand press and measure the pellet infrared spectrum.
Following that, the pellet was withdrawn from the collar and the entire die set was returned
to the desiccator.

Figure 1 : Hand Press KBr Pellet

Data & Results
1. Polystyrene (C8H8)n

Functional Wavenumber Experiment

Molecular Motion
Group (cm-1) Wavenumber (cm-1)
3082.1
C-H stretch 3100.0 – 3010.0 3060.0
Aromatic
3026.0
C-H bend 869.0 – 680.0 700.9
2923.5
Alkene C-H stretch 3000.0 – 2095.0
2849.8

2. Caffeine (C8H10N4O2)

Functional Wavenumber Experiment

Molecular Motion
Group (cm-1) Wavenumber (cm-1)
Aromatic C=C stretch 1600.0 – 1500.0 1548.9
Amine C-N stretch 1350.0 – 1020.0 1025.1
 1073.7
1239.7
1285.9
C=O stretch 1690.0 – 1630.0 1661.6
Amide out of plane
3700.0 – 3500.0 3736.5
N-H stretch

3. Paraffin (CnH (2n+2))

Wavenumber Experiment
Functional Group Molecular Motion
(cm-1) Wavenumber (cm-1)
2924.3
2729.0
C-H stretch 3000.0 – 2095.0
2675.5
Alkene 2403.3
CH2 bend 900.0 – 690.0 722.3
CH3 bend (4 or 1456.0
1470.0 – 1340.0
more) 1377.2

4. Acetophenone (C6H5C(O)CH3)
 Wavenumber Experiment
Functional Group Molecular Motion
(cm-1) Wavenumber (cm-1)
C=O stretch 1690.0 – 1680.0 1682.8
Ketone 1180.8
C-C stretch 1300.0 – 1100.0
1101.8
C-H stretch 3100.0 – 3010.0 3062.1
Aromatic
C=C stretch 1600.0 – 1500.0 1599.3

5. Toluene (C6H5CH3)

Wavenumber Experiment
Functional Group Molecular Motion
(cm-1) Wavenumber (cm-1)
3056.1
C-H stretch 3100.0 – 3010.0
Aromatic 3028.2
C-C stretch 1600.0 – 1500.0 1494.8
Alkyl C-H stretch 2950.0 – 2850.0 2734.6

6. Unknown 1 (CH3CH3OH)
Wavenumber Experiment
Functional Group Molecular Motion
(cm-1) Wavenumber (cm-1)
Alkene C-H stretch 3000.0 – 2095.0 2924.9
O-H stretch 3500.0 – 2500.0 3370.9
Alcohol
C-O stretch 1260.0 – 1000.0 1050.4
7. Unknown 2 (C18H3O2)
Wavenumber Experiment
Functional Group Molecular Motion
(cm-1) Wavenumber (cm-1)
C-H stretch 3000.0 – 2095.0 2925.8
Alkene CH2 stretch 690.0 – 900.0 723.4
CH3 stretch 1340.0 – 1470.0 1435.6
Alcohol O-H stretch 3500.0 – 2500.0 2674.9
C-O stretch 1320.0 – 1210.0 1283.2
Carbocyclic Acid
C=O stretch 1710.0 – 1780.0 1713.2

Discussion
The FTIR machine underwent a background check before the experiment to ensure that it is in
good working order by running a blank spectrum. The equipment was calibrated using a standard
polystyrene film and the calibrated marks are applied to it. It can be shown from comparing IR
spectra that the machine was correctly calibrated and in excellent working order. In order to
identify the compound of unknown 1, the critical bending and stretching frequency of the functional
group was investigated and compared to the IR absorptions for Representative Functional Groups
Infrared Spectroscopy. At a stretching point, O-H were stretched at 3370.9 cm-1, C-O at 1050.4
cm-1. Between ethanol and oleic acid come unknown compounds. Since there was no spectrum
that revealed the presence of the carboxylic acid functional group when we searched for the
functional group of oleic acid, we can infer that ethanol is the Unknown 1 compound. The second
stretch of the spectrum was examined in order to be assured that the chemical is an alcohol. The
molecular motion that was absorbed at wavenumber 2925.8 cm-1 was determined to represent
the C–H stretch. We discovered the C=O stretch at wavenumber 1713.2 cm-1 and the C-O stretch
of carboxylic acid at wavelength 1283.2 cm-1 from the bending and stretching frequency of the
functional group of Unknown 2. O-H Stretch at 2674.9 cm-1 in wavelength. Alkene functional group
of alkenes, C-H stretch, may be found at 2925.8 cm-1, 723.4 cm-1 for CH2, and 1435.6 cm-1 for
CH3. We may infer that unknown 2 is oleic acid due to the presence of the carboxylic acid
compound. The findings lead to the conclusion that the unknowns 1 and 2 are ethanol and oleic
acid.
Conclusion
To conclude, we may infer from the provided IR spectrum graph that the unidentified sample is
ethanol and oleic acid. This result depends solely on the graph's stretching frequency bands,
where the absorbed wavenumber indicated the existence of functional groups for alcohol and
alkane molecules.

Reference

1. IR Absorption Frequencies - NIU - Department of Chemistry and Biochemistry. (n.d.).

Northern Illinois University. https://www.niu.edu/clas/chembio/research/analytical-
lab/ftir/ir-frequencies-table.shtml
2. Lampman, P., Kriz, & Vyvyan. (n.d.). Introduction to. Retrieved November 6, 2019, from
https://www.fkit.unizg.hr/_download/repository/Introduction_to_Spectroscopy_4e_by_P
avia.pdf