EXP 3 Full

ANALYTICAL CHEMISTRY LAB REPORT
EXPERIMENT 3:
FOURIER TRANSFORM INFRARED SPECTROSCOPY
QUALITATIVE ANALYSIS OF ASPIRIN TABLE
GROUP NUMBER
:1
GROUP MEMBERS
: LUQMAN HAKIM BIN ROSLI

CHAN SIN WEI
DEMONSTRATERS NAME
16098
16173
MARSHA DAEYANA BINTI SHAHROM
16587
MOHAMMAD HANIFF BIN MOHD ZAINI
16025
AIN MUNIRAH BINTI YUSOF
16661
INDEX
1 OBJECTIVE
..
2 APPARATUS
..
3 CHEMICAL
..
4 INTRODUCTION
..
5 PROCEDURE
6 FLOW
CHART.
7 CALCULATION AND
RESULT..
8 DISCUSSION
.
9 RELIABILITY AND
MODIFICATION.
10 CONCLUSION
..
OBJECTIVE:
This experiment will measure the absorption of infrared light by salicylic acid and
acetylsalicylic acid. A commercial aspirin tablet containing both of these molecules will
be analyzed and the spectra will be compared.
INSTRUMENTATION:
Fourier Transformed Infrared Spectrophotometer (Model: FTIR-8400S Shimadzu)
MATERIALS:
Polystyrene Calibration Film
KBr (Potassium Bromide)
Salicylic Acid
Commercial Aspirin Tablet
INTRODUCTION:
Infrared (IR) radiation with wavelengths of 700 nm to 50,000 nm is found in the
electromagnetic spectrum between the visible and microwave regions. It can be applied
to the analysis of organic molecules by causing molecular rotation and/or molecular

vibrations (stretching or bending of bonds) in the molecules.
PROCEDURE:
The operating manual and the instruction for the operation of the instrument have been
thoroughly read before beginning the experiment.
A. Preparation of KBr Pellets

In order to measure the absorption of the sample, a transparent sample container
material has been used to infrared radiation. KBr is used since it has excellent
transparency in the IR. Solid samples are measured by grinding the sample into a fine
powder and mixing a small amount of sample powder with powdered KBr.
1. Blank KBr Pellet
a. 200 to 300 mg of KBr was grinded into a fine powder using a mortar and
pestle.
b. The operating instructions were followed to create a KBr pellet.
2. Salicylic Acid in KBr Pellet
a. 200 to 300 mg of KBr was grinded into a fine powder using a mortar and
pestle.
b. 1 to 2 mg sample of Salicylic Acid was also grinded into a fine powder.
c. The Salicylic Acid was added to the ground KBr and mixed by grinding the
mixture.
d. The mixture was pressed into a KBr pellet.
Same procedure is repeated by using Commercial Aspirin tablet as solid sample.
B. Obtain IR Spectra
The instruction on how to use the Fourier Transformed Infrared Spectrophotometer
(FTIR-8400S Shimadzu), had been given by the instructor before the experiment
started. All the spectra were obtained using the following parameters and save all
scans.
Range: 4500 cm-1
Number of Scans: 16
1.
IR Background Spectrum: The background IR spectrum was obtained without a
sample in the instrument.

2. Polystyrene Calibration Film Spectrum:
i. The polystyrene calibration film was placed in the sample holder and obtains the
spectrum at a resolution of 16.0 cm-1.
3.
Blank KBr pellet Spectrum: The blank KBr pellet was placed in the sample
holder and the spectrum was obtained.

4.
Salicylic Acid Spectrum: The salicylic acid/KBr pellet was placed in the sample
holder and the spectrum was obtained.

5.
Commercial Aspirin Spectrum: The aspirin /KBr pellet
sample holder and the spectrum was obtained.
was placed in the
FLOW CHART
DISCUSSION
QUESTION
1. Sketch the main components of an FTIR infrared absorption

spectrophotometer.
The basic components of an FTIR are shown schematically in Figure 1. The infrared
source emits a broad band of different wavelength of infrared radiation. The IR source
used in the Temet GASMET FTIR CR-series is a SiC ceramic at a temperature of 1550
K. The IR radiation goes through an interferometer that modulates the infrared radiation.
The interferometer performs an optical inverse Fourier transform on the entering IR
radiation. The modulated IR beam passes through the gas sample where it is absorbed
to various extents at different wavelengths by the various molecules present. Finally the
intensity of the IR beam is detected by a detector, which is a liquid-nitrogen cooled MCT
(Mercury-Cadmium-Telluride) detector in the case of the Temet GASMET FTIR CRseries. The detected signal is digitised and Fourier transformed by the computer to get
the IR spectrum of the sample gas.
Figure 1: Basic components of FTIR

A common FTIR spectrometer consists of a source, interferometer, sample
compartment, detector, amplifier, A/D convertor, and a computer. The source generates
radiation which passes the sample through the interferometer and reaches the detector.
Then the signal is amplified and converted to digital signal by the amplifier and analogto-digital converter, respectively. Eventually, the signal is transferred to a computer in
which Fourier transform is carried out. Figure 2 is a block diagram of an FTIR
spectrometer.
Figure 2. Block
spectrometer
diagram of an FTIR
The major difference between an FTIR spectrometer and a dispersive IR

spectrometer is the Michelson interferometer.
Michelson Interferometer
The Michelson interferometer, which is the core of FTIR spectrometers, is used to split
one beam of light into two so that the paths of the two beams are different. Then the
Michelson interferometer recombines the two beams and conducts them into the
detector where the difference of the intensity of these two beams is measured as a
function of the difference of the paths. Figure 3 is a schematic of the Michelson
Interferometer.
Figure 3. Schematic of the Michelson interferometer

A typical Michelson interferometer consists of two perpendicular mirrors and a
beamsplitter. One of the mirrors is a stationary mirror and another one is a movable
mirror. The beamsplitter is designed to transmit half of the light and reflect half of the
light. Subsequently, the transmitted light and the reflected light strike the stationary
mirror and the movable mirror, respectively. When reflected back by the mirrors, two
beams of light recombine with each other at the beamsplitter.
If the distances travelled by two beams are the same which means the distances
between two mirrors and the beamsplitter are the same, the situation is defined as zero
path difference (ZPD). But imagine if the movable mirror moves away from the
beamsplitter, the light beam which strikes the movable mirror will travel a longer
distance than the light beam which strikes the stationary mirror. The distance which the
movable mirror is away from the ZPD is defined as the mirror displacement and is
represented by . It is obvious that the extra distance travelled by the light which strikes
the movable mirror is 2. The extra distance is defined as the optical path difference
(OPD) and is represented by delta. Therefore,
=2
It is well established that when OPD is the multiples of the
wavelength, constructive interference occurs because crests overlap with crests,
troughs with troughs. As a result, a maximum intensity signal is observed by the
detector. This situation can be described by the following equation:
=n
(n = 0,1,2,3...)
In contrast, when OPD is the half wavelength or half wavelength add multiples of
wavelength, destructive interference occurs because crests overlap with troughs.
Consequently, a minimum intensity signal is observed by the detector. This situation can
be described by the following equation:
=(n+12)
(n = 0,1,2,3...)
These two situations are two extreme situations. If the OPD is neither n-fold
wavelengths nor (n+1/2)-fold wavelengths, the interference should be between
constructive and destructive. So the intensity of the signal should be between maximum
and minimum. Since the mirror moves back and forth, the intensity of the signal
increases and decreases which gives rise to a cosine wave. The plot is defined as an
interferogram. When detecting the radiation of a broad band source rather than a singlewavelength source, a peak at ZPD is found in the interferogram. At the other distance
scanned, the signal decays quickly since the mirror moves back and forth. Figure
4(a) shows an interferogram of a broad band source.
2. Hand in copies of all spectra acquired during this experiment .
3. Explain why the IR Background spectrum has peaks even though the
sample chamber was empty.
The IR spectrum is usually displayed as per cent transmittance that is how much
of the original IR intensity is left after passing through the sample. In order to calculate
this, we first need to know the IR intensity with no sample, so we run a background.
In the background spectrum, there are strong IR peaks near 3800, 2400, 1600
cm . These peaks are due to the O-H stretch of H2O, the asymmetric stretch of CO2
and the H-O-H bending of H2O, respectively. The H2O and CO2 are present in the air,
which fills the spectrometer. The H2O bands consist of many sharp peaks. These
peaks are the vibrational transitions between different rotational states of H 2O. With a
higher resolution instrument, the CO2 band shows similar rotational splitting, but the
lines are closer together. Rotational splitting is only observed in the gas phase.
Passing a steady stream of nitrogen though the spectrometer can eliminate the H 2O and
CO2 bands. This is called purging the spectrometer.
-1
Even without the CO2 and H2O bands, the background spectrum is much more
intense in the middle than at both ends reflecting the output spectrum of the source:
strong in the middle, but falling off at the ends.
Figure 1.0: A typical FTIR Background Spectrum.
4. Examine the salicylic acid spectrum. Using the structure of salicylic acid, identify the major
peaks in the spectrum.
Table 1 : Typical Infrared Absorption Frequencies
Figure 2: Molecular structure of

Salicylic acid.
From the graph of the infrared
analysis of salicylic acid, the peaks from the
graph are shown below and their
functional group based from table 1
3480.13 : O-H (alcohol functional
group)
3415.19 : O-H (alcohol functional group)
3237.83 : O-H (alcohol functional group)
3011.38 : O-H (carboxylic acid)
2597.99 : O-H (carboxylic acid)
1986.48 : C=C (alkenes)
1921.09 : C=C (alkenes)
1866.29 : C=O
1832.79 : C=O
1662.04 : C=O
1612.67 : C=O
1575.78 : C=C
1443.54 : C=C
1481.70 : C=C
1296.73 : O-C
1245.76 : C-O (phenol)
1209.03 : C-O (phenol)
1152.15 : C-O (phenol)
1028.58 : C-O (phenol)
966.22 : C=C-H
891.26 : C-H
758.47 : O-H ( weak bond)
694.75 : C-H
656.44 : C-H
The major peaks in the spectrum for salicylic acid can be determined by the bonds which are OH with range of around 3500 to 2500 followed by C=O with range of 1800 to 1600.
The range for C=O is not accurate due to impurities within the samples.
5. Examine the commercial aspirin spectrum and determine spectral contributions from
salicylic acid.
Figure 3 : Molecular Structure of Aspirin

From the graph of the infrared analysis of aspirin, the peaks from the graph are shown below and
their functional group based from table 1
3487.78 : O-H
2871.86 : CH3, CH2,CH
2696.74 : C-H
2586.59 : O-H
2094.30 : C=C
1998.92 : C=C
1967.87 : C=C
1756.62 : C=O
1690.42 : C=O
1605.75 : C=C
1457.51 : CH2
1417.36 : CH2
1369.79 : CH2
1303.96 : O-C
1216.86 : O-C
1187.81 : O-C
1091.53 : C-C-C
1012.25 : C-C-C
1036.18 : C-C-C
918.67 : C-H
970.28 : C=C-H
839.32 : alkenes
798.74 : alkenes
755.32 : alkenes
702.40 : alkenes
664.20 : C-H
The spectral contributions of aspirin from salicylic acid based on the spectrum analysis are the
O-H and C=O bond. All the bonds identified are taken in approximation to their respective
frequency due to impurities in the sample while conducting the experiment.

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ANALYTICAL CHEMISTRY LAB REPORT

: LUQMAN HAKIM BIN ROSLI

MARSHA DAEYANA BINTI SHAHROM

MOHAMMAD HANIFF BIN MOHD ZAINI

AIN MUNIRAH BINTI YUSOF

to the analysis of organic molecules by causing molecular rotation and/or molecular

A. Preparation of KBr Pellets

Same procedure is repeated by using Commercial Aspirin tablet as solid sample.

IR Background Spectrum: The background IR spectrum was obtained without a

sample in the instrument.

holder and the spectrum was obtained.

holder and the spectrum was obtained.

Commercial Aspirin Spectrum: The aspirin /KBr pellet

sample holder and the spectrum was obtained.

was placed in the

1. Sketch the main components of an FTIR infrared absorption

Figure 1: Basic components of FTIR

The major difference between an FTIR spectrometer and a dispersive IR

Figure 3. Schematic of the Michelson interferometer

2. Hand in copies of all spectra acquired during this experiment .

Figure 1.0: A typical FTIR Background Spectrum.

Table 1 : Typical Infrared Absorption Frequencies

Figure 2: Molecular structure of

Figure 3 : Molecular Structure of Aspirin

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