Analysis of Polymeric Samples using the Thermo

Scientific Nicolet iS50 FT-IR Spectrometer

Steffany Ann L. Moreno1, Nick Joaquin Rapadas2, Jose Emmanuel G. Rivera3
Department of Mining, Metallurgical and Materials Engineering
University of the Philippines Diliman
Quezon City, Philippines
steffymoreno@gmail.com1, nicko_rapadas@yahoo.com.ph2, jose.emmanuel.g.rivera@gmail.com3
AbstractFourier Transform Infrared (FTIR) spectroscopy is
one of many analytical techniques present for unknown analysis
and characterization. Mostly used in organic compounds, thin
films, gas, liquid, and powder samples, the FTIR provides a wide
variety of data for analysis. An experiment was performed to
determine the effect of sample thickness on the resulting
spectrum as well as to utilize FTIR spectroscopy for unknown
analysis. Two samples of polystyrene of varying thickness (1.5
mil; 3.0 mil) and one unknown sample were subjected to FTIR
spectroscopy analysis. Results showed presence of alkanes and
aromatic compounds on the polystyrene samples whereas,
carbonyl groups were discovered on the unknown sample. The
unknown sample was then determined to be a variant of a low
density polyethylene (LDPE). Furthermore, the resulting
transmittance of infrared rays were observed to be decreasing
while the resulting absorbance of infrared rays were observed to
be increasing with increasing thickness causing an increase in
peak sizes for the 3.0 mil polystyrene sample. Additional analysis
can be done to further pinpoint the compounds present in the
unknown sample.
Index TermsFTIR, polymer, spectroscopy, transmittance,
absorbance.

I. INTRODUCTION
Fourier Transform Infrared or FT-IR spectroscopy is a
technique that uses infrared radiation to generate the molecular
fingerprint of a sample. By this method, infrared radiation that
is passed through the sample is either absorbed or transmitted
(Thermo Nicolet Corporation 2001). A visual representation of
this process is shown in Fig. 1.

Fig. 1. Conceptual diagram of the beam path through a sample (Thermo

Fisher Scientific Inc. 2013)

When infrared radiation hits the sample, the atoms in the

material vibrates and produce a corresponding frequency. In
measuring these infrared frequencies, an interferometer is
utilized. The interferometer is an optical device that produces
a signal containing all the infrared frequencies. However, this
signal cannot be directly interpreted, thus, a means of
decoding is needed. Fourier transformation is employed to
convert this signal into useful information, the spectrum
containing the absorption peaks. These absorption peaks in the
spectrum represent the produced frequencies. Furthermore, the
peak sizes indicate the amount of material present in the
sample. Knowing that materials have unique atomic
arrangement and composition, it is expected that no two
materials will produce the same spectra. The complete process
of conversion from the beam source to the resulting spectrum
is shown in Fig. 2.

Moreno, S.A.L., Rapadas, N.J., Rivera, J.E.G. (2015)

Page 1 of 5

B. Demonstration of equipment operation

Fig. 2. The process of infrared spectroscopy (Thermo Nicolet Corporation

2001)

Due to this capability, FT-IR has been used in several types

of analysis, specifically, in identifying unknown samples. This
analytical technique can determine the amount of components
present in the sample as well as the quality and consistency of
a material (Thermo Nicolet Corporation 2001).
Samples that can be analyzed include powders, thin films,
gas and even liquids. Researchers have employed FT-IR to
determine the bonds present in their samples, verifying the
presence of a specific material. As Materials Engineers, whose
concerns focus on material analysis, this analytical technique
can be utilized.
In this paper, the spectrographs of polystyrene of thickness
1.5 mil, and 3.0 mil, and an unknown polymeric sample will
be analyzed using FTIR spectroscopy. Differences in the
obtained spectrographs and the peaks present in the polymer
samples will be identified. Moreover, effect of the thickness
obtained in the FT-IR spectrograph will also be discussed.

Fig. 3. Thermo Scientific Nicolet iS50 FT-IR Spectrometer

The equipment used in the analysis of the polymeric

samples was the Thermo Scientific Nicolet iS50 FT-IR
Spectrometer. After sample preparation, the samples were
placed in a compartment where the incident beam can pass
through. The background spectrum was obtained to eliminate
noise or unwanted data. Samples will then be scanned to
obtain its respective spectral data. The two known samples
that were analyzed are shown in Fig. 4.

II. METHODOLOGY
A. Sampling Techniques and Sample Preparation
There are three types of analysis based on sample
preparation transmission, reflectance and emission. For the
equipment used in the demonstration, the first two were
discussed. If transmission technique is used, analysis can be
carried out for solids, liquids and gases (King et al. 2004).
Moreover, samples must be in pellet, mull or film form
(Thermo Fisher Scientific Inc. 2013). The obtained spectra for
this kind of analysis provides the percent absorbance or percent
transmission versus the wavenumber.
If reflectance analysis is used, specifically the attenuated
total reflection (ATR), the samples must not react or scratch the
ATR crystal (King et al. 2004). Some of the available ATR
crystals are diamond and germanium (Bruker Optics 2011).
Samples that can be analyzed include homogeneous solids,
coatings, laminates, powders and thin films. ATR is also ideal
for liquid analysis (Thermo Fisher Scientific Inc. 2013). It is
important to note that when reflectance is used instead of
transmission, only the surface of the sample is being analyzed.
Basic sample preparation for solids utilizes Potassium
Bromide (KBr). The solid samples are dried and grounded with
KBr which are then formed into pellets. For liquid samples,
the solution is placed in a liquid cell for measurement. Finally,
for gas samples, KBr windows are placed on each side of the
gas cell (Birkner and Wang 2014).

Fig. 4. Polystyrene Film Samples

Aside from the polystyrene film samples, the spectral data

of an unknown polymeric material was also obtained using the
FT-IR spectrometer.
III. RESULTS AND DISCUSSION
An infrared spectrum acquired using FTIR spectroscopy
serves as a guide in determining the identity of different
materials through the use of the absorption peaks that
correspond to the vibration frequencies of the atomic bonds
present in the material.

Moreno, S.A.L., Rapadas, N.J., Rivera, J.E.G. (2015)

Page 2 of 5

Of the three samples analyzed by utilizing the FTIR

spectrometer, two samples of polystyrene (1.5 and 3.0 mil
thick) were used for demonstration while the third sample was
subjected to unknown analysis. The infrared spectra of the two
polystyrene samples were presented in terms of absorbance v
wavenumbers and transmittance v wavenumbers, as shown in
Fig. 5, 6, 7 and 8.

Fig. 7. Infrared Spectrum of polystyrene with sample thickness=1.5

(Transmittance)

Fig. 5. Infrared Spectrum of polystyrene with sample thickness=1.5

(Absorbance)

Fig. 8. Infrared Spectrum of polystyrene with sample thickness=3.0

(Transmittance)

Fig. 6. Infrared Spectrum of polystyrene with sample thickness=3.0

(Absorbance)

By observing the infrared spectra of the polystyrene

samples it can be seen that the increase in sample thickness
leads to higher intensities for the infrared absorbance which
relates to lower infrared transmittance. A possible reason for
this can be accounted by the increase on the amount of
material present in the thicker sample which consequentially,
leads to more incident infrared rays absorbed and less
transmitted. The change in thickness have affected the
intensity of the peaks observed but, caused no major changes,
except at the 1600-1900 (cm-1) wavelength.

The peaks for the polystyrene samples were found out to be

at wavenumbers 3025-3081, 2849-2923, 1795-1936, 1601,
1372-1490, 678 and 539 cm-1. At 3025-3059 cm-1, indications
that vibrations of the stretch of aromatic H-C= bonds are
present in the polystyrene sample, while at 2849-2923 cm -1 ,
peaks measured indicate presence of H-C-H saturated systems
(alkanes).Moreover, on the 1795-1936, and 1601 cm-1 peaks,
presence of double bonds, C=C were discovered; the peaks at
1372-1490 cm-1 can be associated to the H-C-H bending of the
alkane and might be due to the methyl (1372 cm -1) and
methylene (1448-1490 cm-1) groups present in the polystyrene
sample, while the peaks at 678 and 539 cm -1 indicate the
substitution patterns (out of plane modes) of the polystyrene
sample.

Moreno, S.A.L., Rapadas, N.J., Rivera, J.E.G. (2015)

Page 3 of 5

Minute differences were observed on some peaks for the

polystyrene samples. These can be attributed to background
noise present during testing (e.g. presence of dirt).
The unknown polymer sample was also analyzed with the
FTIR machine, determining its absorbance and transmittance
IR spectra as shown in Fig. 9 and 10.

REFERENCES
[1] Birkner, Nancy, and Qian Wang. 2014. How an FTIR
Spectrometer Operates Development of IR Spectrometers
FTIR Spectrometers, no. 1: 18.
[2] Bruker Optics. 2011. Application Note AN # 79 Attenuated Total
Reflection ( ATR ) a Versatile Tool for FT-IR Spectroscopy
Refractive Index.
[3] King, P.L., M.S. Ramsey, P.F. McMillan, and G. Swayze. 2004.
Laboratory Fourier Transform Infrared Spectroscopy Methods
for Geologic Samples.
[4] Thermo Fisher Scientific Inc. 2013. Introduction to FT-IR
Sample Handling.
[5] n.d. Accessed August 31, 2015.
http://academics.wellesley.edu/Chemistry/Chem105manual/La
b06/lab06.html.

Fig. 9. Infrared Absorbance Spectrum of Sample

[6] n.d. Accessed August 31, 2015.

http://mmrc.caltech.edu/FTIR/FTIRintro.pdf.
[7] n.d. Accessed August 31, 2015.
http://www.chem.ucla.edu/~bacher/spectrocopy/IR1.html.
[8] Thermo Nicolet Corporation. 2001. Introduction to Fourier
Transform Infrared Spectrometry. A Thermo Electron
Bussines. http://mmrc.caltech.edu/FTIR/FTIRintro.pdf.

Appendix:
Fig. 10. Infrared Transmittance Spectrum of Sample

The peak wavenumbers for the sample are at 2944.64 cm -1,

2865.21 cm-1, 1724.12 cm-1, and 961.56-1470.68 cm-1. At
peaks, 2944.64 and 2865.21 cm-1 we can indicate the presence
of saturated systems (alkanes) due to the C-H stretching
modes, while the 1724.13 and 1189.52 cm -1 peaks can be
associated with the presence of a carbonyl group or the
presence of a stretch of aromatic C=C double bonds [5] [6];
The unknown sample could be then classified as a variant of
Low-density polyethylene (LDPE). This is backed up by
presence of a carbonyl group, and a series of double bonds
(polyethylene) present in the sample.
IV. CONCLUSION
By utilizing the Fourier Transform Infrared spectroscopy,
the experiment was able to verify that the thin films used were
indeed polystyrene due to the presence of alkanes and aromatic
compounds. Increasing thickness was also observed to
decrease transmittance resulting in increased value of the
peaks. The unknown sample was also identified by comparing
the acquired spectral data to that of a database. Presence of a
carbonyl group and double bonds suggest the sample to be a
LDPE variant.

Fig. 11. Characteristic peaks for Carbonyl Group-Ketone-Cyclohexanone,

from [6]

Moreno, S.A.L., Rapadas, N.J., Rivera, J.E.G. (2015)

Page 4 of 5

Fig. 12. . Peaks for Polystyrene, from [5]

Moreno, S.A.L., Rapadas, N.J., Rivera, J.E.G. (2015)

Page 5 of 5