Infrared
Spectroscopy (FT-IR)
Infrared spectroscopy is a
technique used to identify various functional groups in unknown substances
through the identification of different covalent bonds that are present
in the compound. By identifying the different covalent bonds that are
present in a compound, you can establish the types of functional groups
present. By comparing the absorptions seen in an experimental spectrum
to the literature absorptions of various functional groups, you can
determine a list of possible identities for the bonds present.
Apparatus

Procedure
FT-IR
spectra may be run from 8 AM to 6 PM Monday-Friday ONLY. If
you want to run one
during another lab, please get the Instructor's
approval.
1. If the software is not already running, double click on the Spectrum
icon to start the acquisition program. When prompted, log in as chem211 with
the password org211.
The instrument is 1. Spectrum One. Do not activate IR assistant. Press
Return or click OK.
2. The program will open and
check the hardware. Then you will see a message which is titled Accessory
Ready Check. It should say System Ready
for Use. You may click the Cancel button.
2A. If you are not the first user and there is a spectrum already displayed,
click on the Delete icon to clear the window for you.
3. Run a background spectrum.
A. Make sure the sample
area is clean
and empty.
B. Choose Scan from the Instrument menu drop down list.
A window titled Spectrum One Scan and Instrument Setup will open. It
has several pages accessed by clicking on the tabs. Choose the Sample
tab and type the name background for Name. Next click
on the Scan tab and, under Options in the middle of the
page, select Background as the Scan type. All other
settings can be left with their default values.
C. Click the Apply button and then the Scan button.
The window will refresh, and soon you will see your background scan
as it is running. A bar in the lower left corner of the screen shows
the progress of the scan. WAIT UNTIL THE SCAN FINISHES. When the scan
is complete, you may be asked if you want to overwrite the old background
scan. Answer Overwrite.
D. Click the Delete icon to clear the spectrum window. The
background scan is not lost!
4. Run a spectrum of your sample.

A. Place a small quantity of your sample on the center of the sample
plate. Swing the pressure arm over the sample and adjust until it touches
the sample. Do not apply pressure yet.
B. Choose Scan from the Instrument menu drop down list.
C. The Spectrum One Scan and Instrument Setup window will open. Choose
the Sample tab and enter a filename for your sample in the Name line.
Fill in the description and comments as you choose. Then click the Apply button.
D. If you have a liquid, go to E. For a solid, click
on the Monitor icon (it looks like a fuel gauge)in the upper
left corner of the window. Then choose the Sample icon (the
second from the left of the three or four blue-ringed icons) and adjust
the pressure by turning the knurled knob on the pressure arm. You will
see a green bar appear in the Force Gauge area. Adjust the pressure
until the green bar almost fills the window. You should have a reading
of 100-120 (above the right end of the bar). Click the Stop button
to stop monitoring, then click the Scan button to start your
scan. You will be able to monitor the progress of your scan as it runs.
E. For a liquid, click the Scan button to start your
scan. You will be able to monitor the progress of your scan as it runs.
5. Analyze and print your data.
A. You can click on the Peaks icon to automatically label your
peaks. Clicking a second time removes the labels. To label peaks
in another way , click on the vertical cursor icon, Vcursr, then drag
the green line over the peak and double click. (If you need to
adjust the threshold, choose Peak Table from the Process menu drop
down list and set a new threshold. Close Peak Table, then click on
peaks twice, (once to remove the old labels and again to show the new)
then click on the box to enlarge the image.)
B. You may zoom a region of the spectrum by dragging a box around
the region of interest and then double clicking inside the box. The
AutoX and AutoY icons will resize the spectrum to full scale.
C. Click on the Text icon to add text to your spectrum.
You have control of the font, and you can drag the text to a new position
after it is written.
D. Click on the Print icon to print a copy of your spectrum.
E. Click the Delete icon to clear the screen for the next user,
or logout if that is appropriate.
6. CLEAN UP! Follow the directions from your instructor to clean
off the sample area. The
following is an example data table which you should use to display
the data given in your infrared spectra.
|
Experimental
Frequencies (cm-1) |
Literature Frequencies
(cm-1)* |
Possible
Peak Assignments
|
|
3320-3300 |
3500-3300
3600-3200 |
N-H stretch: 2o amine
OH stretch: alcohol,
phenol |
|
1730-1710 |
1730-1625 |
C=O stretch: carboxylic
acid, ketone, aldehyde |
(Literature IR
frequency absorptions were taken from Table 1 below)
Table 1:
Principal IR Absorptions for Certain Functional Groups above 1400
cm-1
|
Functional
Group Names
&
Example Compounds
|
Absorption
Ranges Frequency (cm--1) [Look for a single
absorption in these regions unless stated otherwise.]
|
Type
of Vibration
(causing
IR absorption)
|
|
Alkanes:

|
3000-2800
(Note:
The absorptions can be seen a several distinct peaks in this
region.)
1500-1450 |
C-H Stretch
C-H Bend |
|
Alkenes:
|
3100-3000
1675-1600 |
=C-H Stretch
C=C Stretch
|
|
Alkynes:

|
3300-3200
2200-2100
|


|
|
Aromatic
Rings:
|
3100-3000
1600-1580
1500-1450 |
=C-H Stretch
C=C Stretch
C=C Stretch
|
|
Alcohols,
Phenols:

|
3600-3100
(Note:
Phenols MUST have Aromatic Ring Absorptions too.)
(1300-1000)
|
H-bonded
O-H Stretch
(C - O Stretch)
|
|
Ketones:

|
1750-1625 |
C=O Stretch
|
|
Aldehydes:
 |
1750-1625
2850-2800
2750-2700 |
C=O Stretch
C-H Stretch
off C=O
C-H Stretch
off C=O
|
|
Carboxylic
Acids:
|
3400-2400
(Note: This peak always covers the entire region with a VERY
BROAD peak.)
1730-1660
|
H-bonded O-H
Stretch
C=O Stretch |
|
Esters:

|
1735
(1300-1000) |
C=O Stretch
(C - O Stretch) |
|
Ethers:

|
(1300-1000)
|
(C - O Stretch)
|
|
Amines:
Primary

|
3500-3200
(TWO PEAKS!)
1640-1560 |
N-H Stretch
N-H Bend
|
|
Amines:
Secondary
|
3500-3200
(ONE
PEAK!)
1550-1450 |
N-H Stretch
N-H Bend
|
|
Nitriles:

|
2300-2200 |

|
|
Nitro Groups:

(Note:
Both peaks are < 200 cm-1 apart.)
|
1600-1500
1400-1300
|
N=O Stretch
N=O Stretch
|
|
Amides:

|
3500-3100
1670-1600
1640-1550 |
N-H Stretch
C=O Stretch
N-H Bend |
Printable Version of
FT-IR Literature Table |