CHM 260

BASIC INSTRUMENTAL ANALYSIS

LABORATORY SUMMARY WRITTEN

REPORT

EXPERIMET 3
Fourier Transform Infrared Spectroscopy (FTIR)

Name: WAN ARINA SYAKIRAH BINTI WAN RUSLI

ID No.: 2019260774
Programme: CHM 260
Instructor: MADAM SITI NOR HAYATI BT MOHD TARMIZI
 EXPERIMET 3
Fourier Transform Infrared Spectroscopy (FTIR)
A. Pre-laboratory questions

a) Write the molecular formula and draw the molecular structure of cinnamic acid.
 C6H5CH=CHCOOH


b) Using the IR table, answer the following questions.

i. Predict the location of three peaks you might expect from its spectrum.

ii. Indicates bonds were responsible for all the peaks you identified in (i).

Bond Wavelength (nm)

C=O 1760 – 1670 (s)
O-H 3400 – 2500 (b)
C=C 1680 – 1640 (m,w)

B. Post-laboratory questions

a) Explain why a background must conduct before obtaining the sample spectrum.
 The background must conduct before obtaining the sample spectrum because to
ensure to get the data only from the sample and not a spectrum that includes
substances that are usually present.

b) Why ‘neat’ liquids, not an aqueous solution, used on salt plates?

 ‘Neat’ liquids was used on salt plates but not the aqueous solution because the
aqueous solution like water is an ineffective solvent since it dissolves the salt plates
and water emits a broad -OH peak that will obscure many of the other peaks that are
 looking for.
C. Answer the following

1. Briefly explain the observation during the preparation of the KBr pellet.
 Agate mortar containing KBr and benzoic acid with ratio 1:80 was mixed until the
mixture become homogeneous. A hydraulic press gauge was used up to 8500 psi to
compress the pellet. After that, run the FTIR test for KBr pellet for analysis if the KBr
looks clear and thin like a piece of glass.

2. Name of compound analyzed.

 C=O (1760-1670 cm-1), C-O (1320-1210 cm-1)

3. The molecular formula of the compound was analyzed.

 C7H6O2

4. The molecular formula of an unknown compound.

 Unknown number: C-H (sp³) (2960-2850 cm-1), C-H (2860-2800 cm-1)
 C6H12

D. Report summary (1-2 pages)

a) INTRODUCTION
Mid-infrared (IR) spectroscopy is a well-known chemical compound identification and
structural investigation technique. Fourier transform infrared (FTIR) spectroscopy is the
primary infrared (IR) spectroscopy method. Infrared radiation is transmitted through a sample
in IR spectroscopy. The sample absorbs some of the IR radiation and some of it passes
through (transmitted). The resulting spectrum shows the sample's molecule absorption and
transmission, resulting in a molecular fingerprint. To circumvent the limitations of dispersive
equipment, FTIR spectrometry was created. The delayed scanning process was the main
issue. It was necessary to develop a system for sensing all IR frequencies simultaneously
rather than individually. A solution was devised using a fundamental optical apparatus known
as an interferometer. The interferometer generated a one-of-a-kind signal containing all of the
IR frequencies "encoded". Each sample's time element was lowered because the signal was
measured in seconds.
The beam splitter in most interferometers accepts the incoming IR beam and separates it into
two optical beams. A flat mirror that is set in place reflects one beam. The other beam reflects
off a flat mirror with a mechanism that permits it to move a small distance away from the
beam splitter (usually a few millimetres). When exposed to IR radiation, chemical bonds
vibrate at specific frequencies, and they absorb the radiation at frequencies that match their
vibration modes. When the frequency of light absorption is measured, a spectrum is produced
that can be used to identify functional groups and compounds. In the infrared region, some
contaminants have their own distinct bands. Spectral measurements of these bands determine
the amounts of contaminants and their bonding with the host material. The observed
interferogram signal cannot be evaluated directly because the analyst requires a frequency
spectrum, which is a visualisation of the strength at each frequency for identification. FTIR
offers a wide range of applications. The first is nanomaterials analysis. The second is
additives, preservatives, and colourants are all included in the food analysis. The third is
environmental analysis, which examines water, airborne particles, and gases. The fourth is
preserving and repairing our cultural assets, such as paintings, sculptures, ceramics, fossils,
and ivory.

b) METHODOLOGY
First is sample preparation: the KBr method. 80 mg of KBr was took into an agate mortar and
pestle. The solid KBr was ground until it becomes powdered. 1 mg of benzoic acid was added
into the powdered KBr for the ratio 1:80. The mixture was ground until it become
homogenous. The mixture must be finely ground or the mixture will scatter the IR radiation
excessively. The die set was cleaned with acetone. The mixture of benzoic acid and KBr was
put into the die set. Make sure the mixture fills the surface of the die set. The die set was
closed tightly. The die set was put into Hydraulic Press gauge. The Hydraulic Press gauge
was tightened. The Hydraulic Press gauge was pressed until the pressure goes up to 7000 psi.
The air was released and let it rest for 2 minutes. The gauge was pressed until the pressure
goes up to 8500 psi and let it rest for about 1 minute. The pressure was released. The die set
was removed slowly from the Hydraulic Press gauge. The die set was opened. The KBr pellet
that was obtained should appear clear like a piece of glass or transparent disk.
Second is operation of the FTIR. The operating instructions depend on the type of IR
instrument or model available in the laboratory. The plate holder was took out. The KBr
pellet was put into the pellet holder. The holder and plate was slid into the bracket on the
instrument in the sample beam. The spectrum was run by pressing the SCAN button and the
result of IR spectrum was appeared.

c) ANALYSIS
From this experiment, we managed to analyze benzoic acid by using the FTIR. The purpose
of using FTIR was to determine the compounds through examine the spectrum for the present
of absorption peaks based on the IR chart. As we knew, the molecular formula of benzoic
acid is C7H6O2 and the existence functional groups are aromatic rings (C-H, C=C) and
carboxylic acids (C-O, C=O, O-H). Based on the benzoic acid spectrum above, the functional
group presented based on the peaks only carboxylic acids. This indicates the peak was C=O
bond with the wavenumbers, 1760 cm-1 – 1670 cm-1 (s) and C-O bond with the
wavenumbers, 1320 cm-1 – 1210 cm-1 (m). The observed value for C=O is 1677.25 cm-1
meanwhile for C-O is 1288.90 cm-1.

d) CONCLUSION
By using FTIR in this experiment, we were able to carry out a qualitative analysis of an
organic compound like benzoic acid. We can prepare the KBr pellet of an organic compound
by using a solid sample such as benzoic acid into the Hydraulic Press gauge for 7000 psi then
up to 8500 psi. We also managed to identify IR absorption peaks and the corresponding
functional groups of an unknown solid or liquid or powder in which the unknown compound
was cyclohexane which was C-H (sp³) (2960-2850 cm-1), C-H (2860-2800 cm-1). One of the
advantages of using FTIR is the throughput advantage. The FT-IR instrument does not use a
slit to limit the amount of light that reaches the detector. Overall, this means that with an FT-
IR spectrometer, more energy reaches the sample and thus the detector than in a dispersive
spectrometer. The FT-IR's signal-to-noise ratio improves as the signal increases. Higher
signal-to-noise ratios suggest that the instrument will be more sensitive to minor absorptions,
and details in a sample spectrum will be crisper and more discernible. Next is a precision
advantage. The velocity of the moving mirror of an FT-IR spectrometer is controlled by a
laser, which also time the collection of data points along the mirror stroke. Within the
instrument, this laser is also employed as a reference signal. The laser's interferogram is a
continuous sine-wave, a reference for the infrared spectrometer's precision and accuracy. This
reference laser, rather than any external reference material, is used only by well-designed FT-
IR spectrometers. Spectra obtained with an FT-IR spectrometer may be compared with
certainty in this example, whether they were taken five minutes apart or five years apart. A
dispersive infrared system or any system that requires external calibration standards does not
have this capacity. Besides that, there are a few limitations of FTIR. Due to its small size, the
sampling chamber of an FTIR can have several restrictions. The IR beam can also be
obstructed by mounted items and only small things, like rings, can usually be checked. Last
but not least, because certain materials absorb infrared radiation, obtaining a reliable result
may be impossible.
REFERENCES
 Dutta, A. (2017). Fourier transform infrared spectroscopy. Spectroscopic methods for
nanomaterials characterization, 73-93.
 Ismail, A. A., van de Voort, F. R., & Sedman, J. (1997). Fourier transform infrared
spectroscopy: principles and applications. In Techniques and instrumentation in
analytical chemistry (Vol. 18, pp. 93-139). Elsevier.
 Vaughan, T. (2019, July 31). Advantages and Disadvantages of Raman & Fourier
Transform Infrared Spectroscopy (FTIR) in the Gemological Field. AGTA. Retrieved
January 5, 2022, from https://agta.org/advantages-and-disadvantages-of-raman-
fourier-transform-infrared-spectroscopy-ftir-in-the-gemological-field/