Rosabiela Irfa Andina ID : SCME 6236874

Lab Report : Fourier Transform Infrared Spectroscopy

Abstract

The objectives of this experiment are to do measurement by using Fourier Transform

Infrared Spectroscopy (FTIR) and analyze the vibrational peak spectra of four polymers. The
investigation is about the different bonds and functional group with different FTIR spectra
characteristic. The FTIR spectra of sample A was indentified tobe nitrile molecule structure
because it has C  N functional group. The FTIR spectra of sample B C and D were supposed
to be PVC, PP and PE respectively. The implication of this experiment is that different
functional group is the one of the major factor to differenciate each IR spectra.

Introduction

The electromagnetic spectrum is the range of all possible frequencies of

electromagnetic radiation. Electromagnetic radiation has several regions of spectrum that can
be determined by the level of wavelength and also related to frequency and energy.
Frequency is the number of wave cycles that pass through a point in one second which
measured in Hertz. Where, wavelength is the length of one complete wave cycle measured in
cm. Those frequency and wavelength are inversly related (Equation 1).

c
 (1)


Where c is the speed of light that has quatity of 3 x 1010 cm/second. The energy of
particle often referred to as a photon (E in Joules) which related to wavelength and frequency
as follows (Equation 2)

hc
E  h  (2)


Where h is Planck’s constant in 6.6 x 10-34 Joules.second. According to mentioned

equations, Energy is directly proportional to frequency. Therefore, high energy radiation will
have a high frequency. On the other hand, Energy is inversly proportional to wavelength.
That short wavelength will has high energy and vice versa [1]
 Figure 1. Electromagnetic spectrum and infrared region (www.chromacademy.com)

Based on provided spectrum region (Figure 1),  -ray and X-ray become the higest
energy radiation which shows a great energy needed to break bonds in molecule. Whereas,
radio wave have very low energies, only enough to make spin transition in nuclear region and
Infrared region gives significant information about the molecular vibrations [2]. Infrared has
three regions includess near (12820-400 cm-1), mid (4000-400 cm-1) and far (400-33 cm-1)
infrared.

Furthmore, electromagnetic spectrum is being basic study in the techology

development of surface analysis of material. There is variety techniques for characterizing
surface and interface. They are classified in terms of atomic or molecular transition that
provides absorption or emission of photons. Vibrational spectroscopy, a technique to get
information about molcule, set to work by the excitation of vibrational modes of molecular
species and it’s interaction on the surface. Where Infrared spectroscopy (IR) is being one of
the most popular methods to study about molecular vibration. These are correspond to the
excitation of specific vibration modes. Nowdays, the common instrument used is Forier
transform spectrometer then named Fourier-tansform infrared (FTIR) Spectroscopy [3].

Molecules that can be detect in infrared spectroscopy must have specific frequencies
at which they rotate or vibrate corresponding to dicrete energy levels known as resonant
frequencies. Those are detemined by the mass of the atoms, the shape of the molecular
potential energy surfaces and by the associated vibronic coupling. Infrared spectroscopy can
detect interaction of polarity of the chemical bonds of the molecules called dipole moments
[4]. Dipole moment is a quantitative measure of the polarity of a molecule bond which owned
by diatomic molecules containing atoms with different elements named polar molecules.
Dipole moment can be used as distinguisher between molecules that have the same formula
but with different structures [5]. Infrared active molecule must undergo a change of its dipole
moment when vibrating. The simplest modes of vibration that are infrared active are
streching and bending.

The objective of this experiment is to analyze the vibrational properties of four

polymers by measuring and observing the FTIR spectra using FT-IR Spectrometer.
Materials and Methods

FTIR spectroscopy is designed base on interference of radiation between two beams

to get an interferogram. For the last step, the signal is produced as a function of changing
pathlength between the two beams. The two domains of distance and frequency are
interconvertible by the mathematical method of Forier-transformation.

Analog-
Source Interferometer Sample Detector Amplifier computer
to-digital

Figure 2 Basic components of an FTIR spectrometer.

FTIR has several basic components as shown in Figure 2 . The radiation produced by
source is passes trough an interferometer to the sample before reaching detector. By signal
amplification, in which high-frequency contributions have been eliminated by a filter, the
data are converted to digital form using an analog-to-digital converter and transferred to the
computer for Fourier-transformation [6]. The main benefit of FT-IR technique over the
conventional IR is the higher signal-to-noise ratios for spectra recorded for the same
measurement time [7]. It also has high precision of wavenumber kalibration (0.01 cm-1) that
known as Connes advantage. Besides its high wavenumber accuracy, FT-IR utilizes circular
apetures which has a larger area than the linear slits used in grating spectrometers that can
provide higher troughput of radiation[8].

Measurements for four different samples (Figure 1 Appendix A) were carried out by
using FTIR Instrument. Polymer was taken from hand glove, small piece of plastic hose,
pippete tip and syringe pump. Each sample was cut it into a small piace to make easier in
term of positioning them to the sample place. Then twice running for each sample was
collected. As with all FT-IR measurements, an infrared background was collected.

The raw data spectra was plotted by using Origin Pro software to be analyzed. The
plotting result is a graph that shows transmittance (%) vs wavenumber (cm-1) in y and x axis
respectively. Then, we bravely analyzed the graph by determining the peak and comparing
with several references to know various materials.

Result and Discussion

FTIR spectra were recorded in the transmittance mode. The FTIR spectra of A-D
sample are shown in Figure 3A-3D, respectively. These bands can be observed to determine
functional group for make certain the material. The reference and list of the functional gorup
in each peaks also given in Table 1A-1D.
 - Sample A

A
110
-1 Fingerprint region
1683-1614 cm
100

90
Transmittance(%)

80
2237 cm-1
2851 cm-1

2359 cm-1
70 2928 cm-1

1435 cm-1
60 3419 cm-1
1176 cm-1

50

40
4000 3500 3000 2500 2000 1500 1000 500
-1
Wavenumbers(cm )

Figure 3A. The FTIR spectra of sample A

For Figure 3A, a broad band at 3419 cm-1 is assigned to O-H streching. Another peaks
are showed at 2928, 2851, 1614-1683, 1435 and 1176 cm-1 which are correspond to C-H
vibration, CH2, C = C Streching, CH2 Scissoring and C-C streching respectively. The
fascinating peak to be observe are at wavenumber of 2539 and 2237 cm-1 that are concerned
with C  N streching. Hence, Based on C  N functional group, it can be guessed that A
sample contain of nitrile material. Furthmore, The FTIR spectra of A sampla also has similar
shape with nitrile material that has been worked by Sadeghalvaad, et al. [9].

Table 1A. The FT-IR spectrum functional group of sample A

Wave number (cm-1) Functional group name Reference

3419 O - H streching [9]
2928 C-H vibration [10]
2851 CH2 [9]
2359 C  N streching [11]
2237 C  N streching [9], [10]
1614-1683 C = C streching [10]
1435 CH2 scissoring [12]
1176 C-C streching [11]
 - Sample B

B
120

110
-1 -1
2838-2990 cm 1409-1473 cm
100
-1
Transmitance (%)

1038 cm
90

80

70
-1
742 cm
60 -1
958 cm
-1
1124 cm
50
-1 -1
1721 cm -1 1069 cm
1255 cm
40
3500 3000 2500 2000 1500 1000 500
-1
Wavenumbers(cm )

Figure 3B. The FTIR spectra of sample B

According to the Figure 3B, peaks at 2838-2990 are assigned to the C-H streching.
Other characteristic of sample B at 1721, 1409-1473,831, 958 and 742 cm-1 are corresponded
to C =O streching, CH2, CH rocking, Trans CH wagging, C-Cl and –CH=CH- (cis)
respectively. The appearance of C-Cl bending can be use to determine this material to be
specified. Those, corresponds with polyvinyl chloride (PVC). Because the FTIR spectra of
sample B is also match with characteristic of PVC spectra which has been done by Ramesh et
al. in previous work.

Table 1B. The FT-IR spectrum functional group of sample B

Wave number (cm-1) Functional group name Reference

2838-2990 C – H streching [13]
1721 C = O streching [14]
1409-1473 CH2 [15]
1255 CH rocking [13],[14]
958 Trans CH wagging [13],[14]
831 C-Cl [13], [14]
742 -CH=CH- (cis) [15]
 - Sample C

C
105
-1
898 cm
-1
2997-2792 cm
100 1045 cm
-1

95
Transmitance (%)

90
2722 cm-1
-1
1102 cm
85
-1
1166 cm

80 -1
1358 cm

75
-1
1455 cm
70

65
-1
1375 cm
60
3500 3000 2500 2000 1500 1000 500
-1
Wavwnumbers (cm )

Figure 3C. The FTIR spectra of sample C

The characteristic spectra of sample C is shown at 2792-2997 and 2771 cm-1 and
expected to be due to C-CH3. The absorption band at 1455, 1375 and 898 cm-1 are bending
vibration of CH2, C-H and C=CH2 respectively. These peaks are close to the characteristic of
polyprophylene (PP). Wang et al. already reported FTIR spectra for pure polyprophylene
polymer that showspeaks at 3000 for C-H streching and also at 1460 and 1375 cm -1 for C-H
bending. Another report was given by Sarker el al. which exhibited PP peaks at 2841.66-
2955.87, 1465.95 and 1377 cm-1 for C-CH3, CH2 and CH3 bending respectively. Therefore,
with all of this study, it can be assume that sample C is PP polymer.

Table 1C. The FT-IR spectrum functional group of sample C

Wave number (cm-1) Functional group name Reference

2997-2792 C-CH3 [16], [17]
2722 C-CH3 [17]
1455 CH2 /CH3 [17], [16]
1375 C-H bending [18]
898 C=CH2 [17]

- Sample D

The FTIR spectra of sample D is shown in Figure 3D. The chacacteristic of peak of
sample also listed in Table 1D. The peak at 2915-2948 cm-1 are assigned to CH2 asymetric
streching. Where, CH2 symmetric streching group is indicated at wavenumber of 2836-2866
cm-1. In addition, CH3 symmetric group is corresponded to the peak at 1375 and 1357 cm-1.
[19] [20]. This study was well matched with the work that has been done by Muhonjaet al.
They investigated biodegradable polyethylene and reported that the main bands of LDPE
consist of a situated band at 2900 which assignable to CH2 as an asymmetric streching, a
band around 1461-1466 cm-1 revealing a bending deformation [21] . Given the functional
group, it can be concluded that the structure of this polymer has to be polyethylene.

D
110

100

90
Transmittance(%)

-1
2721cm

80 1263 cm
-1

-1
70 1357 cm

2836 cm-1 -1
60 1456 cm
2866 cm-1

50
2948 cm-1 -1
1375 cm
40 -1
2915 cm

3500 3000 2500 2000 1500 1000 500

-1
Wavenumbers (cm )

Figure 3D. The FTIR spectra of sample D

Table 1D. The FT-IR spectrum functional group of sample D

Wave number (cm-1) Functional Group

2915-2948 CH2 asymetric streching [19]
2836-2866 CH2 symmettic streching [19]
2721 C=N
1456 CH2 group bending [20]
1375 CH3 symmetric group [19]
1357 CH3 symmetric group [20]
1263 Secondary alcohol [21]

Conclusion

FTIR spectroscopy is a significant tool for studying molecular structure of material

base on its functional groups. Because, by the functional group we can identify characteristic
of each material. Using FTIR spectrometer, four polymers were identified by using literature
review. The FTIR spectrum of sample A was identified to relate to Nitrile structure. Sample
B was supposed to be PVC molecular structure. In addition, sample C was determined to be
PP and sample D was identified to relate to PE.
 The FTIR signatures of sample A, B, C and D have common peaks around 2900 and
1400 cm -1 that present methylene as functional group. Niitril polymer has different structure
with C  N bonding. Whereas, PVC has C-Cl bonding in its structure. However, the
characteristic of PP, PE and PVC are hard to distinguish by just comparing the peak. Because
those FTIR specra have possibilty to be polystyrene polymer due to their similar FTIR graph.

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Appendix A Pictures of sample A,B,C and D.

A B

C D
Appendix B Product data sheet of materials

PVC
NITRILE
PE