Perkin-Elmer Spectrum One FT-IR Spectrometer

Rehana Rupan, Alana Boyd, Richard Cantoral

St. John’s University, Department of Chemistry, 8000 Utopia Parkway, Jamaica, NY 11439

Abstract Experimental Discussion

In this experiment, a Perkin-Elmer Spectrum One FTIR Spectrometer was used to obtain
infrared spectra of an unknown compound, as well as to compare the effectiveness of
polyethylene and other household plastics as materials for IR sampling cards. In short,
infrared spectrophotometers work by shining a beam of light onto a diffraction prism so that
only infrared light is allowed to exit and strike a sample. The light that passes through this
sample is detected by a sensor and converts transmittance and frequency data into a digital
display. It was found that the unknown compound contained saturated and unsaturated
hydrocarbons, as well as either an N-H bond or a C=O bond. Upon comparing experimental
data to literature, it is hypothesized that the unknown molecule is a ketone; however, an
NMR spectra is needed to verify our hypothesis. It was also found that while household
materials do not exceed the effectiveness of commercial polyethylene sampling cards,
materials such as plastic bags and wrappers do provide a decent inexpensive alternative to
mulls or pellets.
To analyze the unknown compound:
• An empty Attenuated Total Reflectance (ATR) attachment was placed in the instrument
and a preliminary spectra was obtained to assure the instrument was functioning properly
• A solution of the unknown compound was made by dissolving 0.1 g in 10 mL of hexane.
• Using a glass syringe, the ATR attachment was filled completely with the solution.
• An IR spectra was obtained using the system software.
To determine the effectiveness of household materials as IR sample cards:
• 2”x4” pieces of cardboard were cut out.
• A one-inch hole was placed one one-half of the piece of cardboard.
• A variety of different plastics were stretched into a thin layer across the hole.
• A second piece of cardboard was used to seal the “IR sample card”
• Spectra of these cards were obtained using system software.
Looking at the IR spectra in Figure 7:
• We first notice that there is a medium-strong peak at 1600 nm which signifies that we may
have N-H bond or a C=O bond in our molecule.
• We have peak slightly below 3000 which is a sign of saturation (sp3 hybridized
hydrocarbons), while a the peak slightly above 3000 signifies unsaturation (sp2 hybridized
hydrocarbons).
• It is hard to determine from this spectra alone whether there is an N-H or amine bond
because there is a slight peak at around 3400 wavenumbers.
• If we compare this spectra to that of the cyclohexanone, shown below, we see that they
are very similar and both have a slight peak at 3400 wavenumbers

Results
120

Figure 1. Basic set up of an infrared spectrometer. https://www.youtube.com/watch?v=pxC6F7bK8CU Date 100

Accessed 03/29/2017 Figure 7. IR Spectra of 2-hexanone (National Institute of Data and Technology) Date Accessed 03/29/2017

Introduction 80
Looking at the compiled IR spectra in Figures 5:
• Infrared Spectroscopy is an important forensic technique used mainly in organic and • When comparing household plastics which are made of polyethylene, all of the materials
inorganic chemistry to study the bonds of molecules, specifically, the presence of 60
produce a similar spectra with the only difference being the “flatness” of the peaks.
functional groups. • When comparing that to the spectra of commercial polyethylene IR sampling cards, we
see that it does in fact produce a very flat baseline.
% Transmittance

• Infrared spectroscopy relies on the interaction of a molecule with infrared light.

40

• When infrared light is shone through a molecule, the bonds begin to oscillate back and 20

forth.

0
4000 3500 3000 2500 2000 1500 1000 500

Wavenumber (1/cm)
Figure 2. Visualization of a hydrocarbon bond acting as a oscillating spring. https://www.khanacademy.org/science/organic-
chemistry/spectroscopy-jay/infrared-spectroscopy-theory/v/signal-characteristics-wave-number. Date Accessed: 03/28/17 Bottle wrap Saran Wrap

Figure 8. IR Spectra of Polyethylene (L.R. Painter et. al.) Polyethylene is commercially used in IR sampling
• From Hook’s law, we can derive the following equation
Sample for a system with two moving Keyfood Baggie Safety Goggle Wrapper cards because they produce a flat baseline when the fill thickness is monitored. (Wigman, et. al.)
objects connected by a springSample
1 𝑘 Stop n' Shop Plastic Bag Thomas English Muffin Wrapper
𝑣=
2𝜋 𝜇 Conclusion
Ziploc Baggie
• Mathematically, as k increases, v increases; and as m increases, 𝑣 decreases. What can be concluded from Figure 6 is that there are both sp2 and sp3 hybridized
hydrocarbons and there is a double bond somewhere in the molecule. If we were to also
• The %transmittance is more closely related to the dipole moment. We can write the Figure 5. Compiled data of all household plastic IR sampling cards. obtain an NMR of this compound, we would most likely be able to identify its structure.
Sample
Sample
following equation for dipole moment (μ):
In our experiment, while no materials created a better baseline than the commercial
Unknown Sample
𝜇 = 𝛿𝑑 polyethylene (Figure8 ), the Keyfood baggie, Thomas English Muffin wrapper, and Safety
Goggle Wrapper produced a relatively flat baseline. The Stop n Shop Plastic bag produced
100
the worst baseline by far and should not be used.
90

80
References
Hydrophilic Hydrophobic
% Transmittance

70

60 1. L. R. Painter, E. T. Arakawa, M. W. Williams, J. C. Ashley, Optical Properties of Polyethylene:

50
Measurement and Applications, Radiation Research, Vol. 83, No. 1 (Jul., 1980), pp. 1-18.
2. Skoog, Holler, and Crouch “PRINCIPLES OF INSTRUMENTAL ANALYSIS”, 6th ed., pgs. 430-477,
40
2007\
30
3. Harris, “QUANTITATIVE CHEMICAL ANALYSIS”, 9th ed., pgs. 415-425, 2016
20 4. National Institute of Data and Technology, “Infrared Spectra of 2-hexanone”
10 5. https://www.thermofisher.com/us/en/home/industrial/spectroscopy-elemental-isotope-
Figures 3 and 4. The affect of dipole momenta on IR Spectra. Notice the difference in %transmittance at ~1700
wavenumbers. Date Accessed 03/28/2017. 0
analysis/spectroscopy-elemental-isotope-analysis-learning-center/molecular-spectroscopy-
4000 3500 3000 2500
Wavenumber (cm-1)
2000 1500 1000 500
information/ftir-information/ftir-basics.html
6. Oliver J. Rees, “Fourier Transform Infrared Spectroscopy: Developments, Techniques, and
• The shape of the peaks in an IR spectra, allows us to detect hydrogen bonding, Applications” Nova Science Publishers, 2010
Figure 6. IR Spectra of unknown sample in ATR attachment.
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1600 Paoli Pike, West Chester, PA 19380. J. Chem. Educ., 1996, 73 (7), p 677.