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Infrared Spectroscopy
Infrared (IR) Spectroscopy is an analytical method that measures the
absorbance of a select band of electromagnetic radiation by a sample. The
wavelength of radiation that is absorbed is characteristic of different types of
chemical bonds. The graphical representation of the absorption of the
electromagnetic radiation by the sample makes an IR spectrum.
Organic chemists use infrared spectroscopy as a means of identifying
various types of bonds within in a molecule which determine the functional
groups present or absent. This information is used to determine the structure
of compounds. IR is usually used in combination with other techniques,
especially nuclear magnetic resonance (NMR) spectroscopy.
In this class you will learn how to interpret an IR spectrum and how to
operate a Perkin-Elmer and/or Nicolet infrared spectrometer. During this
experiment you will obtain an IR spectrum of an unknown compound and use
this information to identify the functional groups present and select the
identification of the material from a list of possible materials.
PRE-EXPERIMENT ASSIGNMENT
Study this chapter of the manual, the lecture notes on the Chemistry
Department web site, the “Sample IR Spectra” posted on the web site and the
appropriate section in your lecture textbook. Complete the take home
assignment relating to Infrared. This will be due at the very beginning of the
lab period.
A major part of this lab will be in operating an Infrared Spectrometer.
Your instructor will explain and show you how to do this. Since all the steps
involve operation of equipment, a pre-lab notebook procedure does not need to
be written. It will however be very important for you to write down in your
notebook all of the possible unknown compounds from the on-line notes. If you
do not have this information, it will be very difficult for you to successfully
determine the identity of your unknown material and points will be lost. The
notebook however will not be graded. In lieu of these points, an in-class
problem set will be assigned.
Quizzes given after the experiment has been performed may also include:
Safety Precautions
All of the compounds you will take IR spectra of in this experiment are at
least slightly toxic and flammable. Wash your hands after conducting the
experiment.
Infrared radiation is relatively (but not completely) harmless. The safety
instructions on the IR spectrometer say “Do not stare into beam,” because long
exposures to IR radiation can be damaging.
EXPERIMENT
Handle salt plates with care. The salt plates are very sensitive to
moisture and will break easily. Each pair costs approximately $25. If you are
the first student, remove the jar containing the salt plates from the desiccator.
(A desiccator is a low humidity vessel.) Remove two salt plates from cotton
envelope. Place the two salt plates on a Kim-Wipe. Clean plates by placing a
few drops of acetone on each salt plate, then wiping clean with Kim-Wipe.
Throw Kim-Wipe away. Place 1-2 drops of unknown liquid on one salt plate.
Cover with other salt plate. Carefully place in sample holder. Take sample to IR
to obtain spectrum.
Obtaining the IR spectrum
Remove salt plates from sample holder. Place salt plates on Kim-Wipe.
Place a few drops of acetone on each salt plate. Using a new Kim-Wipe, rub
each salt plate with the acetone. If another student is waiting to run the
spectrometer, help them go through the process. If you are the last user,
replace each salt plate in a separate cotton envelope. Place each envelope
within the plastic jar. Place the plastic container back in the desiccator.
Throw away any used Kim-Wipes.
Cap your unknown sample. Replace unknown sample in its designated spot
within the unknown sample container.
POST-EXPERIMENT ASSIGNMENT
Complete the datasheet and turn in before leaving class. Ensure your IR
spectrum is stapled to the datasheet. Turn in the white notebook pages from
your lab notebook. Staple multiple sheets together. Tear off rough edges.
Prepare for the IR portion of the next quiz. Remember that you may be
asked questions on anything you should have learned from assigned readings,
pre-experiment lecture, or doing the experiment.
≡ 2100-2300
(Triple Bond)
C≡N 2200-2300 weak sharp
C≡C-H 2100-2260 very weak sharp
= 1620-1800
(Double Bond)
C=O 1650-1800 strong
C=C 1620-1680 medium, sharp
2500-3500 -O-H (carboxylic acid) Very broad (over ~ 500 cm-1), often
looks like distorted baseline, can be
above 3000-1.
1620-1680 C=C (alkene, aromatic ring) Check to see if you have a sp C-H
unsaturated stretch at >3000cm-1 (if
not, it is completely substituted)
~1600 -NH2 (bending 1o amines and Only if you have corresponding N-H
amides) peak at 3200-3500 cm-1 (otherwise
this peak may be mistaken for C=C).