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MINDANAO UNIVERSITY OF SCIENCE AND TECHNOLOGY C.M. Recto Ave., Lapasan, Cagayan de Oro City INFRARED

MINDANAO UNIVERSITY OF SCIENCE AND TECHNOLOGY C.M. Recto Ave., Lapasan, Cagayan de Oro City

INFRARED SPECTROSCOPY

Activity No. 1

Submittted by:

John Mark C. Saburao

BS Chem- 3H1

February 25, 2016

OBJECTIVES

At the end of this experiment, the students should be able to:

1. Study the instrumentation of a Fourier Transform-Infrared (FT-IR) spectrometer

2. Identify and familiarize the components of a FT-IR spectrometer

3. Understand the theory and concept behind infrared spectroscopy as one of the analytical methods used in chemistry

THEORETICAL BACKGROUND

One of the techniques used in determining the structure of an organic compound is infrared spectroscopy. In infrared spectroscopy, the functional groups that are present in an organic compound are determined. Infrared spectroscopy involves the interaction of molecules with electromagnetic energy. Thus the concept of radiant energy and electromagnetic spectrum is very important when dealing with spectroscopic techniques involving infrared spectroscopy. Visible light, X rays, microwaves, radio waves, ultraviolet rays, gamma rays and so forth are all different kinds of electromagnetic radiation. Collectively, they make up the electromagnetic spectrum which is arbitrarily divided into regions, with the familiar visible region accounting for only a small portion. The visible region is flanked by the infrared and ultraviolet regions. When an organic compound is exposed to a beam of electromagnetic radiation, it absorbs energy of some wavelengths but passes or transmits energy of other wavelengths. Irradiating the sample with energy of many different wavelengths and determining which are absorbed and which are transmitted; the absorption spectrum of a compound can be measured. The energy a molecule gains when it absorbs radiation is distributed over the molecule in some way. With infrared radiation, the absorbed energy causes bonds to stretch and bend more vigorously. The stretching and bending of the molecules provide structural information when interpreted. The instrument used in infrared spectroscopy is the Fourier transform infrared (FT-IR) spectrometer. FT-IR provides useful information when identifying unknown substances, determining the quality or consistency of a sample, and determining the amount of the components in a mixture.

METHODOLOGY

A. Liquid Sample Preparation

The IR cell is removed from the storage desiccator. Then, the crystal holder is carefully disassembled by unscrewing the plastic (male) piece. The pieces are placed on a clean paper towel strip. After which, the crystals are removed by inverting the metal part of the crystal holder. The crystals are placed in a clean paper towel. Then, the teflon spacer in the metal holder may be replaced if necessary. Following that, place about one gram of the salt crystals into the metal holder. Then, using a clean pipet, a drop of the sample is placed in the center of the crystal in the metal holder. The other crystal is squarely placed on top of the first crystal to spread the liquid into a film. After that, the cell is reassembled by screwing the plastic holder piece. Next, the cell mount is placed in the IR spectrometer. Then, the cell is placed on the cell mount. Lastly, the IR spectrum of the sample is obtained.

B. Solid Sample Preparation

The IR cell is removed from the storage desiccator and placed on a clean paper towel strip. Then, in a 1-dram vial, a very small volume (<0.5 mL) of a slightly concentrated solution of the solid sample in a volatile solvent is prepared. After which, 1-2 drops of the solution is placed in the center of one of the NaCl plates. The solvent is allowed to evaporate from the crystal for several minutes. The solvent evaporation can be hastened by waving the hand back and forth over the crystal. Following that, the salt crystal is placed into the metal holder with the sample on top. The second crystal is not required any more. Then, the cell is reassembled by screwing the plastic holder piece. After that, the IR cell is placed in the IR spectrometer and the spectrum of the sample is obtained.

C. Gas Sample Preparation

A gas sample is introduced into the gas cells by connecting one of the taps to a vacuum pump and opening it to evacuate the cell. After closing the tap, the other tap is connected to the sample and opened to fill the gas cell with the gas sample. Then, the internal pressure is set from several tens of Torr to 760 Torr. When filling the cell, the pressure is adjust by using a pressure gauge or if there is no pressure gauge, a sampling system with a manometer is used. Then, the gas cell, manometer, and vessel containing the sample is connected. The taps are opened to

evacuate the gas flow line, and then the third tap is closed, followed by the first tap. The fourth tap is gradually opened to allow the sample to flow into the gas cell. The manometer is then observed and the fourth tap is closed when the appropriate pressure is reached. Finally, the second tap is closed and the gas cell is removed.

DISCUSSION

The basic components in an FT-IR system are sample, mirror, IR source, interferometer, detector and computer. The same types of radiation sources are used for both dispersive and Fourier transform spectrometers. Infrared energy is emitted from a glowing black-body source. This beam passes through an aperture which controls the amount of energy presented to the sample. The interferometer divides radiant beams, generates an optical path difference between the beams, then recombines them in order to produce repetitive interference signals measured as a function of optical path difference by a detector. The interferometer produces interference signals, which contain infrared spectral information generated after passing through a sample. The beam enters the interferometer where the “spectral encoding” takes place. The resulting interferogram signal then exits the interferometer. An interferometer consists of three active components: a moving mirror, a fixed mirror, and a beamsplitter. The two mirrors are perpendicular to each other. The beamsplitter is a semi-reflecting device and is often made by depositing a thin film of germanium onto a flat KBr substrate. Radiation from the broadband IR source is collimated and directed into the interferometer, and impinges on the beamsplitter. At the beamsplitter, half the IR beam is transmitted to the fixed mirror and the remaining half is reflected to the moving mirror. After the divided beams are reflected from the two mirrors, they are recombined at the beamsplitter. Due to changes in the relative position of the moving mirror to the fixed mirror, an interference pattern is generated. The beam enters the sample compartment where it is transmitted through or reflected off of the surface of the sample, depending on the type of analysis being accomplished. This is where specific frequencies of energy, which are uniquely characteristic of the sample, are absorbed.The resulting beam then passes through the sample and is eventually focused on the detector. For an easier explanation, the detector response for a single-frequency component from the IR source is first considered. This simulates an idealized situation where the source a modulated monochromatic beam from a helium neon (He-Ne) laser.The measured signal is digitized and sent to the computer where the

Fourier transformation takes place. The final infrared spectrum is then presented to the user for

interpretation and any further manipulation. The figure below shows a typical Fourier transform

infrared spectrometer.

shows a typical Fourier transform infrared spectrometer. Fig.1. Fourier transform infrared spectrometer REFERENCES

Fig.1. Fourier transform infrared spectrometer

REFERENCES

Board of Trustees of Northern Illinois University. (2007). Sample preparation for FT-IR - NIU - Chemistry Analytical Lab. Retrieved February from http://www.niu.edu/ ANALYTICALLAB/ftir/samplepreparation.shtml

D. L. Pavia, G. M. Lampman, and G. S. Kriz, in Introduction to Spectroscopy: A Guide for Students of Organic Chemistry. Harcourt Brace College Publishers, Fort Worth (1996).

Derry, P., & Barron, A. R. (2000). OpenStax CNX. Retrieved from http://cnx.org/contents/uie DnVBC@20.16:vdl5g77_@1/IR-Sample-Preparation-A-Practical Guide

Mitra, S. (Ed.). (2003). Sample Preparation Techniques in Analytical Chemistry. Hoboken, New Jersey: John Wiley & Sons.