Experiment #8.

Determination of the IR absorption spectrum of a liquid sample and

solid
Initial Questions:

1. What is IR spectroscopy? What is it mainly used for?

2. How is IR of liquid samples performed?
3. How can you detect impurities in IR spectra?
4. Can you use water as solvent? Why, why not?
5. How can you use a solvent in the IR spectrometry?

Infrared spectrometry is extremely useful for qualitative assessments of organic

compounds and for deducing molecular structures from their functional groups of both
organic compounds as inorganic.
In the qualitative analysis, infrared spectroscopy can be used for the identification of
pure substances or for the absorption, localization, and identification of impurities. To
locate an impurity in a substance, one needs to make a comparison of the spectrum of
the substance being studied and a sample of the pure substance. Impurities cause
additional absorption bands that appear in the spectrum.
The IR also is used in quantitative analysis, the main field of application of this type of
analysis is in quantifying atmospheric pollutants that come from industrial processes.
Material and reagents
Problem samples: 1 and 2.
NaCl cells for Spectrophotometer
Gloves, 1 dropper
Hexane
acetone
Cyclohexane
Decane
Benzene
Pentanol or other alcohol
Formic acid or another carboxylic acid

Experimental procedure
Liquid
Turn on the Spectrophotometer and allow it to equilibrate for approximately 10 minutes.
Choose a pure organic compound that is in a liquid state in terms of pressure and
temperature.
Place the cell over the sample holder in the Spectrophotometer and choose the option
Run background.
Place a small drop of the sample over a NaCl cell, place the Teflon separator, and over
this other NaCl cell.
Place the sample holders and select the Run Sample option.
Save the spectrum at the appropriate option.
Remove the sample-holding and clean the NaCl cells with acetone
Solid
Choose a pure inorganic compound that is in solid state under normal pressure and
temperature conditions.
One milligram of the finely ground test sample is well mixed with 100 mg of KBr powder
previously dried at 100 °C for at least one hour. The mixture should be made in an
agate mortar. Then, with a spatula, carefully pour enough sample to cover the matrix
and cover the surface uniformly. If needed, you can tap the mold. It is then covered with
the plunger and taken to a press to obtain a transparent disc. When it reaches the
required pressure, it is left for about 2 minutes and decompresses slowly to prevent the
tablet from breaking. The disk is pulled out of the press, and the plunger is gently slid,
separating the pad and gently moving it into the sample holder.

Lab report
Assign group bands in the spectra. What are the samples given by the instructor? How
do the spectra compare to the standards found online? Comment on the impurities in
the samples.