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AS245: Bachelor in Science Applied Chemistry

Title: Analysis of Aspirin Tablet


Course: Spectrochemical Methods of Analysis
(CHM580)
Name: Mohamad Nor Amirul Azhar b. Kamis
Matrix no:

2014647344 (AS245 3S)

Date of experiment: 18th March 2015


Date of submission: 29th May 2015
Group members: 1. Nurnailah bt. Noorazlan
2. Nor Amirah bt. Ahmad Azuan
3. Noramira bt. Saad
It is my responsibility as a student of UiTM to adhere
to truthfulness and avoid dishonesty, fraud or deceit
of any type in connection with write up and conduct
of this experiment.
Signature:__________
Date:

TITLE:

Analysis of aspirin tablet by using Fourier Transform Infrared (FTIR).

ABSTRACT:
Background spectrum was scanned to avoid the interference from moisture or water
and carbon dioxide. Three standards of caffeine, penachetin and acetylsalicylic acid
(ASA) were scanned by using FTIR. The aspirin sample was analysed and followed
by scanning and unknown (unknown A) to determine the functional group of all of
them. All of the standards and sample were analysed by using pelleting method
which is the mixing between the solid of standard with KBr to make a pellet to be
analysed. The bonds appear in each of standards, sample and an unknown were
tabulated in tables. It is proven that the unknown is the salicylaldehyde (C 7H6O2) with
transmitted signals at 2834.15cm -1 (C-H aldehyde) and 1496.87cm -1 (Ar-COH for ring
C=C).

INTRODUCTION:
Aspirin is widely used as an analgesic or pain reliever and for reducing fever. It is
also helps to prevent the heart attacks, strokes and blood clot formation in people at
risk of developing blood clots. Aspirin is also known as acetylsalicylic acid is an
aromatic compound that contains both a carboxylic acid functional group and an
ester functional group. Aspirin is a weak monoprotic acid that only slightly soluble in
water and acidic solution. It can form hydrogen bonds with polar water molecules.
Aspirin is more soluble in alkaline solution, so it is readily dissolves in the duodenum
which is first part of human intestine. The infrared absorption only occurs when the
IR radiation interacts with the molecules that undergo change in dipole moment as it
vibrate or rotate and when the incoming IR photon has sufficient energy for the
transition to the next allowed vibrational state. Large net dipole moment change will
cause stronger intensity of the band in IR spectrum. FTIR is a simultaneous analysis
of the full spectra range using interferometry. The main optical components of FTIR
spectrometer are, source, interferometer, beamsplitter, laser and detector. The
sample can be in solid, liquid or gas. There are two types of sample handling

techniques for solid sample that are by pellet or mull. For this experiment, the pellet
sample handling was used.
OBJECTIVES:
1. To perform KBr-handpress method.
2. To obtain IR spectra of penachetin, caffeine, acetylsalysilic acid (ASA), aspirin
and an unknown.

EXPERIMENTAL:
1. Preparation of pellet:
a. Solid penachetin was mixed with KBr solid in the ratio of 1:99 in the pestle.
b. The mixture was grinded until the shiny solid appear.
c. The mixture then was inserted into the handpress die to form the pellet.
d. The pellet was taken for analysis.
e. Other pellets were done by same procedure for caffeine, ASA, aspirin and
the unknown.
RESULT:
a. IR band assignments of acetylsalicylic acid (aspirin)
Bonds
Name
C=O
C-O
C=C
O-H
C-O

Notes
Carboxylic acid
Carboxylic acid
Aromatic ring
Carboxylic acid
Carboxylic acid

Wavenumber (cm-1)
Theoretical
Experimental
1780-1710
1754.6
1300-1000
1188.26
1600-1580
1606.1
3300-2500 (broad)
2872.63
1320-1210
1306.67

b. IR band assignments of caffeine


Bonds
Name
C-N
C-O

Notes
Amine, aromatic
amides

Wavenumber (cm-1)
Theoretical
Experimental
1360-1250
1359.92
1680-1630
1660.47

c. IR band assignments of penachetin


Bonds
Name

Notes

Wavenumber (cm-1)
Theoretical
Experimental

N-H
C=O
C-O

2 amide
Amide
Ether

About 3300
1680-1630
1300-1000

3286.72
1659.47
1245.61

d. IR band assignments of unknown A (C7H6O2-salicylaldehyde)


Bonds
Name
C-H
Ar-COH

Notes
Aldehyde
Aldehyde (for ring

Wavenumber (cm-1)
Theoretical
Experimental
2860-2800 (weak)
2834.15
1600-1450
1496.87

C=C)

DISCUSSION:
Acetylsalicylic acid is also known with the name of aspirin, so that the spectrum
between ASA standard and aspirin is mostly the same. Any subtle different may be
due to the solid that may contaminate by impurities from other sources. The
functional group of ASA is the carboxylic acid, so that the signals are based on the IR
absorption of carboxylic acid functional group. Caffeine contains two functional
groups that are amine and amide, so that it shows a signal for both functional
groups. Same goes to penachetin that has functional group of amide and ester.
Penachetin shows 2 weak signals for amide functional group at 3286.72cm -1 and
1659.47cm-1, and a sharp and strong signal for C-O ether at 1245.61cm -1. The IR
band for salicylaldehyde (unknown A) shows the broad aldehyde functional group
signal at 2834.15cm-1 for C-H aldehyde and at 1496.87cm -1 weakly for Ar-COH
aldehyde for ring C=C. Aspirin sample should have the same spectrum as the
standard ASA because it contains same molecular structure and of course the same
functional group. Any different between the spectrums may due to the interferences
from environment or contamination of the sample.
It is necessary to run the background spectrum before starts with analysing other
compounds. This is because the background spectrum contains the water molecules
in the air moisture and also the carbon dioxide in the environment of the analysing,
so that when the compounds spectra are analysed, the water and CO 2 will be
deducted to get only the signal for the particular compound. The FTIR instrument
uses the laser as the internal calibrator, so that there is no need to do the calibration

by using the standard polystyrene in order to know the efficiency of the instrument
like in the dispersive IR instrument.

CONCLUSION:
The spectrums for all standards, sample aspirin and the unknown A were obtained
by running the FTIR and the unknown A is proven to be the salicylaldehyde with the
respective bonds observed in the spectrum.

REFERENCES:
1. Aspirin (acetylsalicylic acid), Retrieved April 22, from
http://www.ausetute.com.au/aspirin.html
2. F. J. Holler, D. A. Skoog, S. R. Crouch (2007), Principles of Instrumental
Analysis 6th ed.), United States, Brooks/Cole Cengage Learning.
3. A. Chan (2002), Synthesis and Analysis of Acetyl Salicylic Acid, Retrieved
April

22,

from

http://www.joshstaiger.org/amychan/Literary/Lab%20Three

%20Report%20Aspirin.pdf
4. V Renganayaki* S Srinivasan and S Suriya, Vibrational Spectroscopy
Investigation on Aspirin Using Semi-Empirical Calculations, Retrieved April 22,
from http://sphinxsai.com/2012/july_sept12/Chem/pdfchem/CT=23%28983990%29%20JS%2012.pdf