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INFRARED SPECTROSCOPY

INFRARED SPECTROSCOPY. Basic concepts of FT-IR spectroscopy. IR spectroscopy is the study of the interactions between infrared electromagnetic energy and matter, and allows for qualitative and quantitative measurements of samples. What is infrared light?.

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INFRARED SPECTROSCOPY

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  1. INFRARED SPECTROSCOPY Basic concepts of FT-IR spectroscopy IR spectroscopy is the study of the interactions between infrared electromagnetic energy and matter, and allows for qualitative and quantitative measurements of samples.

  2. What is infrared light? The electromagnetic spectrum can be divided into specific regions, including: Gamma rays, X-Rays, Ultraviolet, Visible, Infrared, Microwave and Radio.

  3. For convenience of applications and instrumentation, the infrared spectrum is divided into near-, mid-, and far-infrared radiation. The most commonly used region is the mid-infrared. Why can infrared light be used? If infrared light energy is absorbed by a sample, it will cause an excitation of the sample‟s molecular vibrations.

  4. This excitation causes the amplitude of chemical bonds to change. It is this change that is measured in infrared spectroscopy. What can you measure with infrared light? IR spectroscopy can be used to analyse samples from all three states of matter –it can be used to analyze gasses, liquids, and solids. Almost all compounds (whether they be organic or inorganic) absorb various portions of infrared light.

  5. Specifically, only chemical bonds that have a dipole moment that changes as a function of vibrations are capable of absorbing infrared light. What is the basic principle of infrared spectroscopy? IR-active bonds produce peaks Every different type of chemical bond that absorbs infrared light naturally vibrates at a specific frequency. Small variations result in peak position and height allow for differentiation. IR spectrum can serve as a compound‟s fingerprint.

  6. The mid-infrared, approximately 4000–400 cm−1 (2.5–25 μm) may be used to study the fundamental vibrations and associated rotational-vibrational structure. Vibrational transitions are responsible for this type of spectra where vibrational stretchings or bendings which result in a net change in dipole moment are IR active.

  7. Symmetrical stretching Antisymmetrical stretching

  8. Rocking Scissoring Twisting Wagging + - + +

  9. Gas Phase Infrared Spectrum of Formaldehyde, H2C=O

  10. Practical IR spectroscopy The infrared spectrum of a sample is recorded by passing a beam of infrared light through the sample. When the frequency of the IR is the same as the vibrational frequency of a bond, absorption occurs. Examination of the transmitted light reveals how much energy was absorbed at each frequency (or wavelength).

  11. FTIR Sampling Modes

  12. Transmission: Sample Preparation for IR IR Cast Films -for solid powders and polymers and non volatile solvents • Dissolve in a volatile solvent or melt. • Apply liquid to an infrared transparent window, allow to dry/solidify. • With luck and skill, could get film neither too thick nor too thin

  13. Transmission: Mulls • Mulls -For powders which could not be dissolved, or would not melt and flow. • Sample ground in a agate mortar with a Mulling Agent. • Mulled sample applied to pair of infrared windows as a capillary film. • With skill and luck, could get a mull that was not too thin or thick, properly ground, and did not react with mulling agent or windows.

  14. Transmission: Pressed Pellets For solids and powders. Sample ground “talcum powder fine”, mixed with finely ground NaCl or KBr powder at ~1% w/w sample/salt. Salt must be absolutely dry. Salt may react with sample (ion exchange). Mixture placed in die, compressed under several tons of pressure to form an infrared transparent pellet. With skill and luck, a clear pellet that was not too thick or thin, and not cloudy or hazy (from large sample particles) would be formed.

  15. Transmission: Gas Analysis Gases much weaker infrared absorbers, use longer path-length to increase absorbance signal intensity.

  16. Attenuated Total Reflectance (ATR) For liquids (organic & aqueous) and solids, especially polymers. Infrared beam internally reflects through the crystal, interacting with sample in contact with the crystal surface.

  17. Fourier transform infrared (FTIR) spectroscopy is a measurement technique that allows one to record infrared spectra. There is an alternate method for taking spectra (the "dispersive" or "scanning monochromator " method), where one wavelength at a time passes through the sample. The dispersive method is more common in UV-Vis spectroscopy, but is less practical in the infrared than the FTIR method.

  18. An interferogram from an FTIR measurement. The horizontal axis is the position of the mirror, and the vertical axis is the amount of light detected. This is the "raw data" which can be Fourier transformed to get the actual spectrum.

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