4.2: IR Spectroscopy - Chemistry LibreTexts

Infrared Optical Materials and Handling

While it is all well and wonderful that substances can be characterized in this fashion one still has to be able to hold the substances inside of the instrument and properly prepare the samples. In an infrared spectrometer (Figure \(\PageIndex{1}\))

the sample to be analyzed is held in front of an infrared laser beam, in order to do this, the sample must be contained in something, consequently this means that the very container the sample is in will absorb some of the infrared beam.

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Figure \(\PageIndex{1}\) An example of a modern benchtop FT-IR spectrometer (Varian Corp.)

This is made somewhat complicated by the fact that all materials have some sort of vibration associated with them. Thus, if the sample holder has an optical window made of something that absorbs near where your sample does, the sample might not be distinguishable from the optical window of the sample holder. The range that is not blocked by a strong absorbance is known as a window (not to be confused with the optical materials of the cell.)

Windows are an important factor to consider when choosing the method to perform an analysis, as seen in Table \(\PageIndex{1}\) there are a number of different materials each with their own characteristic absorption spectra and chemical properties. Keep these factors in mind when performing analyses and precious sample will be saved. For most organic compounds NaCl works well though it is susceptible to attack from moisture. For metal coordination complexes KBr, or CsI typically work well due to their large windows. If money is not a problem then diamond or sapphire can be used for plates.

Table \(\PageIndex{1}\) Various IR-transparent materials and their solubilities and other notes. M. R. Derrick, D. Stulik, and J. M. Landry, in Scientific Tools in Conservation: Infrared Spectroscopy in Conservation Science. Getty Conservation Institute (1999).
Material Transparent Ranges (cm -1) Solubility Notes
NaCl 40,000 - 625 H2O Easy to polish, hygroscopic
Silica glass 55,000-3,000 HF Attacked by HF
Quartz 40,000-2,500 HF Attacked by HF
Sapphire 20,000-1,780 - Strong
Diamond 40,000-2,500 and 1,800-200 - Very strong, expensive, hard, useless for pellets
CaF2 70,000-1,110 Acids Attacked by acids, avoid ammonium salts
BaF2 65,000-700 - Avoid ammonium salts
ZnSe 10,000 - 550 Acids Brittle, attacked by acids
AgCl 25,000-400 - Soft, sensitive to light.
KCl 40,000-500 H2O, Et2O, acetone Hygroscopic, soft, easily polished, commonly used in making pellets.
KBr 40,000-400 H2O, EtOH Hygroscopic, soft, easily polished, commonly used in making pellets.
CsBr 10,000-250 H2O, EtOH, acetone Hygroscopic soft
CsI 10,000-200 H2O, EtOH, MeOH, acetone Hygroscopic, soft.
Teflon 5,000-1,200; 1,200-900 - Inert, disposable
Polyethylene 4,000-3,000; 2,800-1,460; 1,380 - 730; 720- 30 - Inert, disposable

Proper handling of these plates will ensure they have a long, useful life. Here follows a few simple pointers on how to handle plates:

  • Avoid contact with solvents that the plates are soluble in.
  • Keep the plates in a dessicator, the less water the better, even if the plates are insoluble to water.
  • Handle with gloves, clean gloves.
  • Avoid wiping the plates to prevent scratching.

That said, these simple guidelines will likely reduce most damage that can occur to a plate by simply holding it other faults such as dropping the plate from a sufficient height can result in more serious damage.

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