INTRODUCTION

The experiment used Fourier Transform infrared spectroscopy (FTIR) to get absorbance
spectra of several organic compound in this experiment. The absorption of IR-radiation is
used to measure distinctive vibrational frequencies in FTIR. Although there are a number of
peaks, only the most extreme ones are relevant to the component you're testing. The acquired
data sets were then subjected to Principal Component Analysis to remove superfluous
information. The PCA aids in the discovery of strongly linked factor combinations in spectra
from collections of data. PCA Scores were utilized to identify the unknown compound by
determining which oil's PCA Scores most closely matched the unknowns. PCA scores are
compared to each other to identify groupings of distinct components. Clustering in PCA plots
can occur in either specific spots or elongated areas, as long as each component has a distinct
cluster from the others.

OBJECTIVE
- To identify IR absorption peaks and the corresponding functional groups of a
compound
- To prepared KBr pellet of an organic compound
- To carry out a qualitative analysis of organic compound using FTIR.

APPARATUS
Pellet

CHEMICALS
Benzoic acid
Unknown (solid/liquid/powder)
PROCEDURE

A. Sample preparation for FTIR (Reflectance)

Solid samples must first be ground finely before use.
1. The spectrum of benzoic acid was run using the Reflectance method.
2. We obtained an unknown powder from our instructor and ran the spectrum.

B. Operation of the FTIR

The operating instruction depend on the type of IR model available
Instrument : Fourier Transform Infrared Spectrometer (FTIR)

Attenuated Total Reflection (ATR)

1. The Attenuated Total Reflection (ATR) was placed inside sample compartment.
2. All the windows are closed to the sample compartment windows.
3. Acetone was rinsed before placed the sample on top of the Single Reflection Crystal
Plate at Sampling Area of the crystal.
4. For powder film sample : we clamped the Pressure tip.

C. Operation procedure
1. Sample accessory was placed in sample compartment. The mixture was sitted for 10
minutes to complete the reaction.
2. The FTIR was connected to the electric supply and switched on until the status
indicator glowed in green and laser indicator glowed in yellow.
3. The parameters were set in the Measurement dialog window.
4. The sample accessory was chosen and we checked the signal for MIR_ATR.XPM.
5. We acquired a background spectrum by clicking background single channel.
6. The sample description was renamed and placed in spectrometer sample
compartment to be measured.
7. After that, click the graph for peak picking and choose start interactive mode.
8. Saved and download the file. 
9. Lastly, print out the graph.
10. Repeat the step  2 until 11 by using an unknown compound. 
RESULTS/DATA

i) Benzoic Acid

FREQUENCY FREQUENCY
BOND COMPOUND TYPE
RANGE TYPE

C-H alkenes 3080-3020(s) 3071.66

O-H Carboxylic acids 3000-2500(b) 2981.30-2554.84

N-H amines 1650-1580(m) 1618.94-1582.68

C=C Aromatic rings 1600,1500(w) 1496.63

C-H alkanes 1470-1350(v) 1453.67-1420.90

C-N amines 1340-1020(m) 1323.81-1026.62

C-H alkenes 1000-675(s) 999.77-683.70

C-H alkynes 700-610(b) 665.98-617.26

ii) Unknown

BOND COMPOUND TYPE FREQUENCY FREQUENCY

RANGE TYPE

C-H Aromatic rings 3100-3000(m) 3153.37-2862.06

C=O Aldehydes, ketones, carboxylic 1760-1670(s) 1715.84-1662.45

acid, esters

C=H Aromatic rings 1600,1500(w) 1586.50-1508.86

C-H alkanes 1470-1350(v) 1463.63-1264.07

C-O Alcohols, ethers, carboxylic 1260-1000(s) 1198.04-1121.63

acids, esters

C-H Alkenes 1000-675(s) 1025.59-958.33

C-H Alkenes 1000-675(s) 858.37-731.72

 Unknown compound is Vanillin

DISCUSSIONS

The study of molecular chemical structure and the conformity of identities of organic and
inorganic substances is known as Fourier Transform Infrared Spectroscopy (FTIR). By
offering descriptions of the substance's molecular structure, this approach aids in the
differentiation of functional groups and the definition of covalent bonding. F'TIR creates a
continuous set of fingerprints for the various chemical compounds that make up a human,
which is especially valuable for identifying organic materials (carbon hydrogen, oxygen, and
nitrogen). The specimen is transformed into a KBr pellet before the FTIR analysis. The
results obtained from the experiment utilizing Fourier Transform Infrared Spectroscopy
(FTIR) are different. The first chemical under investigation is powdered benzoic acid. The
resulting results are displayed in the spectrum. The spectrum peaks with wavenumbers
greater than 3500 are static, with severe peaks moving beginning at 1678.94 and ending at
665.98. The next substance being tested is referred to as unknown. From wavenumber 3500
and above, the spectrum peaks are static, but they begin to respond at wavenumber 1662.45
and continue until wavenumber 631.09. When tested using FTIR instrument, it was
discovered that benzoic acid and the unknown substance have distinct reactions.
PRE-LABORATORY QUESTIONS

For cinnamic acid :

1. Write the molecular formula = C9H802
2. Draw the molecular structure

3. Based on the molecular structure and using the table provided (or any IR Correlation
charts available) :
i) Predict the location of three peaks you might expect from its spectrum
ii) Indicate what bonds were responsible for all the peaks you identified in (i).

Frequency Bond

2500-3400 OH

1682 C=O

1629 C=C

QUESTIONS

1. Explain why a background spectrum must be run before obtaining the sample
spectrum
- This ensures that you just receive data from your sample, rather than a spectrum
that includes additional substances that are usually present.

2. Why must ‘neat’ liquids and not aqueous solutions be used on salt plates?
- ‘neat’ liquids is easier in preparation because no mixing is required whereas the
aqueous solution will dissolve the salt plates.
CONCLUSION
We may conclude from this experiment that with FTIR, we can do a qualitative analysis of an
organic compound such as benzoic acid. We can also determine the IR absorption peaks and
functional groups of an unknown solid, liquid, or powder.

REFERENCES

Bruker Optics. (2020, March 10). Attenuated Total Reflection (ATR) Mode - Advantages for

FT-IR Spectroscopy. AZoM.Com. https://www.azom.com/article.aspx?

ArticleID=5958

Rizal, T. (2006). EXPERIMENT 3 : FOURIER TRANSFORMED INFRARED. Prezi.Com.

https://prezi.com/-f96_3pqwfl_/experiment-3-fourier-transformed-infrared/

Wikipedia contributors. (2021, September 18). Benzoic acid. Wikipedia.

https://en.wikipedia.org/wiki/Benzoic_acid