Polymer Properties (EBT 326)

Exp. 4: FTIR

EXPERIMENT 4
Determination of Functionality in Polymeric Materials

1.0 OBJECTIVE
1.1 To investigate the functional groups of polymeric materials and polymer blends.
1.2 To find out how FTIR spectroscopy differentiate types of blends.
2.0 INTRODUCTION
An infrared spectrum represents a fingerprint of a sample with absorption peaks which
correspond to the frequencies of vibrations between the bonds of the atoms making up the
material. Because each different material is a unique combination of atoms, no two
compounds produce the exact same infrared spectrum. Therefore, infrared spectroscopy can
result a positive identification (qualitative analysis) of every different kind of material. In
addition, the size of peaks in the spectrum is a direct indication of the amount of material
present. With modern software algorithms, infrared is an excellent tool for quantitative
analysis. [1]
On the other hand, there are two types of IR spectroscopies, dispersive spectroscopy
and fourier transform infrared spectroscopy (FTIR spectroscopy). The major difficulty from
using dispersive spectroscopy is slow scanning process, hence FTIR spectroscopy was
developed to overcome dispersive spectroscopy weakness. The difference between both of
them is the placement of interferometer. The interferometer cut the rambling process of
dispersive spectroscopy and produces a unique type of signal which has all of the infrared
frequencies encoded into it. This convenient makes the signal can be measured quicker than
dispersive spectroscopy [2]. Thus the time process is cut out in FTIR spectroscopy. The
interferogram is then converted by the fourier transform software into a spectrum of
transmittance against wave number [3]. Most importantly, FTIR spectroscopy has a single
beam, whereas dispersive spectroscopy usually has a double beam. Assuming there is no
change in atmospheric conditions throughout the experiment, this does not cause a problem.
However, for highly sensitive work and experiments which take a long time, changes in
infrared absorbing gas concentration can severely affect the results. Therefore, in these cases,
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when using an FTIR spectroscopy, it is necessary to purge the instrument of CO2 and water
vapour using an infrared transparent gas such as nitrogen.
There are also some advantages while using FTIR spectroscopy compared to
dispersive spectroscopy [1]:

It is a non-destructive technique
Provide the spectrum much more rapidly than the dispersive spectrometer.
It provides a precise measurement method which requires no external calibration,

more accurate in accuracy and improved in resolution

Have ability to work over a greater range of infrared intensities
It can increase speed, collecting a scan every second
It can increase sensitivity one second scans can be co-added together to ratio out

random noise
It has greater optical throughout
It is mechanically simple with only one moving part

There are several types of sample preparation, for solid specimen we could use attenuated
total refection (ATR). If the sample is in powder form we could use KBr as a fastener for our
powder sample and pressing the mixture under high pressure. Nujol Mull also can be used for
sample in powder form, it involves grinding the compound with mineral oil (Nujol) to create
a suspension of the finely ground sample dispersed in the mineral oil.

Figure 1: FTIR spectroscopy sample analysis process

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Figure 2: FTIR spectroscopy layout

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3.0 MATERIALS AND EQUIPMENT

3.1 Materials of polymer and polymer blends
3.1.1 Pure/Virgin Polypropylene (PP)
3.1.2 Alumina (Al2O3)
3.1.3 7 wt% PP/Al2O3 Composite

Figure 3: Al2o3 composite, alumina powder, PP

3.2 Fourier transform infrared spectroscopy (FTIR spectroscopy)

Figure 4: FTIR spectoscopy machine

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3.3 Tweezer

Figure 5: tweezer

3.4 Attenuated Total Reflectance (ATR) sample holder

Figure 6: ATR for solid and powder sample

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4.0 PROCEDURE
4.1 Raw materials without other preparation were prepared.
4.2 Sample holder (ATR) was cleaned and then attached to the FTIR machine (Spectrum
RX)
4.3 Spectrum V5.3.1 software was launched on the desktop.
4.4 For calibrate sample holder, Instrument button was selected, then scan background
and review, overwrite and lastly delete background scan.
4.5 Using a tweezers, solid sample was placed on the sample holder and the sample has to
nicely cover the sample holder surface.
4.6 The solid sample was indented and locked by the anvil of sample holder.

Figure 7: The sample was locked by the anvil

4.7 Instrument button is clicked, then for scanning the sample, scan sample was
selected, at scan parameter ATR end was setting to 650cm-1 and ok. The sample
was scanned by selected scan sample. When the scan complete dialog box
appeared, the scan was finally completed.
4.8 The spectrums were collected and saved to avoid data loss.
4.9 For analysis, process was selected from menu, as for broaden the peaks, smooth
was clicked and the view for viewing the peaks. Lastly the peaks were labeled by
selecting label peak.
4.10 The anvil was lifted and the sample was removed by using tweezers.
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Polymer Properties (EBT 326)

4.11
4.12

Exp. 4: FTIR

The steps 4.4-4.9 were repeated for other two samples.

The sample holder (ATR) was cleaned and removed from FTIR machine.

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Exp. 4: FTIR

5.0 RESULT AND DISCUSSION

Figure 8: composite, alumina, PP spectrum analysis

Figure 8 is the infrared spectrum of the samples that we had been conducted in this
experiment. The Y-axis was showing the percentage of the transmitted infrared light of the
compound inside the specimen and the X-axis showing their wavelength (). There were three
conditions and three spectrums showing on this figure, pure polypropylene, alumina, and
PP/alumina composite.
In plain view, we can see from the composite spectrum is more smooth compared to the
alumina and PP spectrum. Composite which has combination of two other material; alumina and
PP shows few smooth peaks compared to alumina and PP which have many peaks which means
it has many several functional groups inside it.

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Exp. 4: FTIR

Table 1: Highest, intermediate and lowest peak values of three samples

Highest peak (cm-1)

Intermediate peak (cm-1)

Lowest peak (cm-1)

PP

2914.67

997.89

3426.16

Alumina

837.35

1537.35

2926.58

Composite

2923.44

1456.54

1657.29

Sample

The highest peak, 2914.67 cm-1 for pure PP was at based on Table of Characteristic IR
Absorptions [Appendix] meaning that in this peak pure PU has CH stretch which is functional
group of alkanes. While the intermediate peak was in 997.89 cm-1 which means it has =CH bend
and belongs to alkenes functional group. And as the lowest peak of pure PP with frequency of
3426.16 cm-1 has OH stretch and Hbonded which is functional group of alcohols and phenols.
For the alumina, the highest peak has frequency of 837.35 cm-1 which has CCl stretch
bond and functional group of alkyl halides. With frequency of 1537.35 cm-1 the intermediate
peak has NO asymmetric stretch and belongs to nitro compounds functional group. And the
lowest peak has frequency of 2926.58 cm-1 and belongs to alkanes functional group that has CH
stretch bond.
As for 7 wt% PP/Al2O3 composite, it is a composite with combination of both other
samples; PP and alumina which make the composite has smoother spectrum compared to the
main combination materials. Having the highest peak frequency in 2923.44 cm-1 almost same as
the highest peak of PP and lowest peak of alumina, the peak has CH stretch bond and functional
group of alkanes. Meanwhile the intermediate peak has frequency of 1456.54 cm-1 has alkanes
and CH bend bond. Lastly the lowest peak frequency is 1657.29 cm-1 has C=C stretch which
belongs to alkenes functional group.

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6.0 CONCLUSION
Based on the experiment that has been conduct, we can prove that the functional group of
polymeric materials and polymeric blends can effect the structure pattern of infrared
spectrum of the material tested. We can see the effect through the value of peak on every
spectrum line graph that obtain from the FTIR spectroscopy machine.
7.0 REFERENCES
[1]
Dr Norzilah Abdul Halif. Fourier Transform Infrared Spectroscopy (FTIR),
Universiti Malaysia Perlis, Perlis, 2015. [Lectures]. Available: UniMAP Portal,
http://portal.unimap.edu.my [accessed on 3 Nov. 2015].
[2]
Mrs Anis Sofia Sufian and Dr Mohd Firdaus Omar, Laboratory Manual for
Polymer Properties, Universiti Malaysia Perlis, Perlis, 2015. [Lectures]. Available: UniMAP
Portal, http://portal.unimap.edu.my [accessed on 1 Nov. 2015].
[3]
Chemical Organization Colorado (2003). IR Chart [Online]. Available:
http://orgchem.colorado.edu/Spectroscopy/specttutor/irchart.html [Accessed Nov. 6, 2015].
[4]
Available: http://mmrc.caltech.edu/FTIR/FTIRintro.pdf [Accessed Nov. 6, 2015].

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8.0 APPENDIX

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