FT-IR Instrument

Components

Source
Michelson Interferometer
Sample
Detector

Sources
Black body radiators
Inert solids resistively heated to 1500-2200 K
Max radiation between 5000-5900 cm-1 (2-1.7
m), falls off to about 1 % max at 670 cm-1 (15
m)
Nernst Glower cylinder made of rear earth
elements
Globar- SiC rod
CO2 laser
Hg arc (Far IR), Tungsten filament (Near IR)

Michaelson Interferometer
1014 Hz is too fast for the rapid changes in
power to be directly measured as a
function of time.
Can not measure the FID signal directly
Interferometer creates a replicate
interference pattern at a frequency that is a
factor of 1010 times slower
104-105 Hz can be measured electronically

f = (2vm/c)10-10vm = 1.5 cm/s

Michaelson Interferometer

Beam splitter
Stationary mirror
Moving mirror at constant velocity
Motor driven Micrometer screw
He/Ne laser; sampling interval, control
mirror velocity

Stationary mirror

HeNe laser

Beam Splitter

Source
Moving mirror
PMT

Sample

Detector

Sample
Sample holder must be transparent to IR- salts
Liquids
Salt Plates
Neat, 1 drop
Samples dissolved in volatile solvents- 0.1-10%

Solids
KBr pellets
Mulling (dispersions)

Quantitative analysis-sealed cell with

NaCl/NaBr/KBr windows

Detector
Transducers
The heating effect of radiation

Thermal transducer- black body, small, very low

heat capacity- T=10-3 K, housed in vacuum,
signal is chopped
Thermocouples
Two junctions of dissimilar metals, An and Bi
One is IR detector, one is reference detector
Potential difference that develops in proportional to
T; detection of Ts of 10-6 K is possible

FT-IR detectors
Pyroelectric tranducers (PTs)
Pyroelectric substances act as temperaturedependent capacitors
Triglycine sulfate is sandwiched between two
electrodes. One electrode is IR transparent
The current across the electrodes is
Temperature dependent
PTs exhibit fast response times, which is why
most FT instruments use them

Photoconducting transducers
Thin film of a semi-conducting material
IR radiation promotes non-conducting electrons
to a higher energy conducting state.
The voltage drop across the thin film is a
measure the Power of the IR beam.
PbS for near IR can be operated at RT
Hg/Cd/Te can be used in the mid-IR and far IR,
but must be cooled to 77 K
Superior response characteristics
Great for GC-IRs

Setting up an experiment
Factors you can control
Spectral Resolution
Number of scans averaged
These combine to determine the overall time required
to collect a spectrum
Signal/Noise ratio N1/2
If S/N ratio is 3 for 1 scan, you can expect the S/N to
increase to 30 if you collect and average 100 scans

Selectivity
Offers much more selectivity that UV-vis
spectroscopy
Absorption peaks are narrow in comparison and
the energies of the absorption bands are unique
for sets of functional groups
Thus qualitative information is readily obtained
from IR spectra
Correlation charts and compilations of IR spectra
for unknown matching
But IR spectra do not have the specificity that
NMR spectra or electron impact mass spectra
tend to exhibit

Sensitivity
This is perhaps the major shortcoming of
this technique when compared to
fluorescence, or especially mass
spectrometry
However, Beers law type analysis are
possible and fairly routine using FT-IR
Detection limits are in the ppm range (M)

ATR

Attenuated total reflectance

More dense media to less dense media
Complete reflectance
Evanescent wave
Penetrates several micrometers
Diamond tip
sample
IR beam