Experiment 3: Fourier Transform Infrared Spectroscopy (FTIR)

Download as pdf or txt
Download as pdf or txt
You are on page 1of 4

EXPERIMENT 3

Fourier Transform Infrared Spectroscopy (FTIR)

A. Pre-laboratory questions

a) Write the chemical formula for cinnamic acid and sketch the molecular structure.

Molecular Formula: C9H8O2


Molecular Structure:

b) Answer the following questions using the IR table.


i. Predict the locations of three peaks in its spectrum that you would expect.

Bonds Wavenumber, 𝑐−1


O−H 3200 – 2500 (b)
C=C 2250 - 2100 (w)
C=O 1780 – 1660 (s)

ii. Indicates that bonds are to blame for all of the peaks you found in the graph
(i).
• O−H is bond of carboxylic acid and happened at peak of 3200-
2500𝑐−1.
• C=C bond is aromatic ring happened at peak of 2250-2100𝑐−1.
• C=O bond is carbonyl group that happened at peak of 1780-
1660𝑐−1.

B. Post-laboratory questions

a) Explain why a background spectrum must be obtained before the sample spectrum
can be obtained.

Because it is possible to ‘subtract' the background spectrum from the sample's


measurements to acquire the true value, the background spectrum must be run
before collecting the sample.

b) Why are ‘neat' liquids used on salt plates rather than an aqueous solution?

On the plates, ‘neat' liquids must be used because they are easier to prepare because
no mixing is required. The salt plates will dissolve in the watery solution.
C. Answer the following

i. Describe the observation made during the manufacture of the KBr pellet in a
few words.

1 g or solid KBr was weighed and dried for 2-3 hours at 110 ℃. Next, 1 mg of
benzoic acid and 80 mg of KBr was grinded together using pestle and mortar
until it become a powder and homogenous. Then, put the mixture inside the
die set and tightly close it. Next, put it into Hydraulic Press gauge and press it
until it goes to 7000 psi. Let it rest for 2 minutes before continue to 8500psi.
The KBr pellet is ready after it was rest for 1 minutes.

ii. Examined compound's name

The name of compound that was analysed is benzoic acid.

iii. The compound's molecular formula was examined.

Benzoic acid
Molecular formula: C7H6O2

Acetone
Molecular formula: C3H6O

iv. An unknown compound's molecular formula

The unknown formula is acetone. Its molecular formula is C3H6O

D. Objective

The objective of this experiment is to perform a qualitative analysis of an organic


compound (such as benzoic acid) and detect IR absorption peaks and the
corresponding functional groups of an unknown solid.

E. Introduction

The measurement techniques for obtaining infrared spectra are known as FTIR
spectroscopy. When the frequency of infrared light travels via a monochromator and
the IR light is steered by an interferometer, it records the amount of energy absorbed.
Polyatomic covalent compounds' IR spectra are frequently exceedingly complicated,
with several absorption bands. Both qualitative and quantitative analysis have been
carried out using IR spectroscopy. An organic compound's IR spectrum has a distinct
fingerprint that distinguishes it from the spectra of other compounds.

F. Procedure

Preparation of Samples for IR Analysis


i. The KBr method
Solid sample and KBr solid were obtained from the desiccator and were
weighed 1 gram each. Then it was dried in the oven for about 2-3 hours at
110℃. 1mg of benzoic acid and 80 mg of KBr was ground using an agate
mortar and pestle for it become powder. After that, the two sample were
mixed for a ratio of 1:80 and grind until its homogenous.
ii. Making the KBr pellet
The die set was removed from the box and cleaned with ethanol. The die set
was closed tightly and put into the hydraulic press gauge until the pressure
goes up to 7000 psi. Then the air was released and it let it rest for 2 minutes
before continue it until pressure goes up to 8500 psi. A clear piece of glass
was obtained and put into a pellet holder for analysis.
iii. Preparing Liquid Samples (neat liquid) using a Salt Plate
‘Neat liquid’ sample was used. 1 or 2 drops of the liquid sample were put on
the plate and cover it with another plate. The entire sandwich was placed in
the IR salt plate holder and cover with a hold-down plate. 2 nuts were put on
the posts of the holder and it was spinning gently to hold the plates with an
even pressure. The holder was slide into the instrument and run the spectrum.
iv. Sample Preparation for FTIR (Reflectance)
The spectrum of benzoic acid was run using the Reflectance method.
After that, an unknown (solid, liquid, powder) obtained from the
instructor and run it in the spectrum.

G. Result and Data

Compound Wavenumber (cm-1) Bond


Benzoic Acid 1. 2570 O-H
2. 1280 C-O
3. 1680 C=O
Unknown 1. 1580 C=O
2. 1520 C=C

H. Discussion

In this experiment, we made a KBr pellet of an organic chemical (benzoic acid) and
used Fourier Transform Infrared Spectroscopy, FTIR, to do a qualitative study on the
organic compound. We may also determine the absorption peak and the related
functional group of an unknown utilising this method of analysis. The KBr pellet was
first made by grinding 80mg KBr and 1mg benzoic acid into a powder and
homogeneous mixture. After that, a piece of pellet was obtained by pressing it with a
Hydraulic Press gauge. Thermo/Nicolet 380 FTIR was used as the FTIR instrument,
and the benzoic acid was run first using the reflectance method. We determine
acetone, or propanone it to be carbonyl based on the references. It has a similar
spectrograph, with a peak between 1580 cm-1 and 1520 cm-1.

By comparing the benzoic acid to the benzoic acid from the reference. The
wavenumber and the peak have a striking resemblance. The region of the stretching
vibration of C=O bonds lies at the peak of 1680 cm-1. Aside from that, the OH
bonding is corroborated by the C- O bond, which can be found at the peak of 1280
cm-1and also at the peak of 2570 cm-1. Acetone was discovered to be the unknown
chemical component.

I. Conclusion

In conclusion, we perform a qualitative analysis of an organic compound (such as


benzoic acid) and detect IR absorption peaks and the corresponding functional
groups of acetone.

You might also like

pFad - Phonifier reborn

Pfad - The Proxy pFad of © 2024 Garber Painting. All rights reserved.

Note: This service is not intended for secure transactions such as banking, social media, email, or purchasing. Use at your own risk. We assume no liability whatsoever for broken pages.


Alternative Proxies:

Alternative Proxy

pFad Proxy

pFad v3 Proxy

pFad v4 Proxy