SPECTRA OF SOLIDS
Introduction:
Mulling is a technique used to prepare solids for infrared analysis. Good results are
obtained by this method only if the average particle size of the solid sample is 1 or 2
microns. Therefore, it is necessary to grind the sample.
The most common mulling agent is mineral oil. Mineral oil is used because it does
not have a lot of absorbance in the infrared range. It may be advantageous to take a
spectrum of plain mineral oil so the peaks that are caused by the oil can be differentiated
when running a sample.
Purpose:
The purpose of this experiment is to obtain the infrared spectrum of a solid
prepared as a mull in mineral oil.
Equipment / Materials:
mullite or agate mortar and pestle Samples:
mineral oil benzoic acid
NaCl windows citric acid
Pasteur pipet and bulb talc (baby powder)
safety gloves acetylysalicylic acid (aspirin)
salicylic acid
sodium bicarbonate (baking soda)
solid unknowns
Safety:
Always wear safety glasses and an apron in the lab.
Always wear gloves when handling the samples and sodium chloride plates.
IR-II-1
Procedure:
1. Place 10 to 15 mg of one of the samples in a mortar.
2. Break up the solid and distribute it over the surface of the mortar by lightly grinding
with the pestle.
3. Grind the sample with a vigorous, hard, back and forth motion with the pestle until it
becomes firmly caked on the sides of the mortar and quite glossy in appearance.
4. Add a small drop of mineral oil to the mortar with a pipet.
5. Grind the sample until all the material is suspended in the mineral oil. It may be
necessary to add another drop of mineral oil.
A note on sodium chloride cells:
Sodium chloride dissolves in water. Consequently, great care must be taken to
ensure that no water or moist materials come in contact with the NaCl cells. For this
reason all cells are to be stored in a desiccator at all times. Always clean the cells
before and after use. Wipe off the sample with a tissue or paper towel and clean
thoroughly with acetone and allow to dry. A spectra of the clean sodium chloride
cells can be run to ensure their cleanliness.
6. Place one of the sodium chloride cells into the cell holder.
7. Transfer the mull from the mortar to the surface of the sodium chloride cell.
8. Place the other sodium chloride cell on top of the sample and smear the two together,
making sure the whole surface area between the both cells is covered and no bubbles
are present.
9. Place the cell holder into the instrument and run a scan of the sample.
10. Clean the sodium chloride cells with acetone and store in a desiccator.
11. If time permits, repeat procedure using an unknown sample.
IR-II-2
Name_______________________________
Name_______________________________
Period______________________________
Date________________________________
SPECTRA OF SOLIDS
Data Table:
List and Identify the major peaks.
Unknown No:_____________________
Major Peaks (cm-1) Functional groups
________________ ________________
________________ ________________
________________ ________________
________________ ________________
________________ ________________
Identity of Unknown:________________
Attach Spectrum
Questions:
1. Why was it necessary to obtain a spectrum of mineral oil?
2. Why was the mineral oil used?
IR-II-3
SPECTRA OF SOLIDS
TEACHER NOTES
Lab Time: 45 minutes
Preparations:
Time: 10-15 minutes
T: Make one set of equipment and materials available to each group with an
instrument.
T: Turn on the instrument at least 10 minutes before the lab.
V: The IR and any other materials are available from the van as requested.
Answers to Questions:
1. Why was it necessary to obtain a spectrum of mineral oil?
The mineral oil spectrum was taken to use as a background to compare the
sample spectrums to.
2. Why was the mineral oil used?
The mineral oil was used because it dissolved the sample into a medium in which
it could be analyzed, but would not dissolve the salt plates.
Considerations:
It takes approximately 10 minutes for each group to prepare and run their sample.
If two sets of NaCl cells are available, one group can be preparing their sample while
another is using the IR. The remainder of the lab time is used in analyzing the collected
spectrum.
It is recommended to run a spectrum of mineral oil ahead of time or have the
students run the spectrum, so that the peaks due to mineral oil can be disregarded in the
analysis.
IR-II-4
Substances can be identified either by comparing spectra to a library of pre-run
spectra or by determining the functional groups present and matching to possible
structures of the substance.
The IR Practice Activity could be used prior to or in combination with this lab. In
addition, this lab could be used to verify the synthesis of aspirin.
Reference:
R. Hannah and J. Swinehart, Experiments in Techniques of Infrared
Spectroscopy. Perkin-Elmer Corporation, Infrared Applications
Laboratory, September 1974.
IR-II-5
