Fourier Transform

Infrared Spectroscopy
(FTIR)
Presented by:
Dr. Jyoti
A.P. Chemical Engineering
Deptt.
Basic theory of FTIR Spectroscopy
Infrared radiation
• Fourier Transform Infrared (FTIR) Spectroscopy
• FTIR spectroscopy
The mass spectrometer(MS) is an instrument that serves for establishment of
the molecular weight and structure of both inorganic and organic compounds,
and the identification and determination of analytes in complex mixtures.
The MS is an instrument capable of producing a beam of ions from sample
under investigation, separating these ions according to their mass-to charge (m/z)
ratios and recording the relative abundances of the separated ion species as a
mass spectrum. The ion-currents corresponding to the different species are
amplified and either displayed on an oscilloscope or a chart-recorder, or are
stored in a computer. The peak intensities are plotted as ordinates, in arbitrary
units or normalized with respect to the most important peak, which is assigned a
value of 100.
Infrared
Designation Abbreviation Wavelength Wavenumber
[μm] [1/cm]
Near Infrared NIR 0.78 - 3 12800 - 3333
Mid Infrared MIR 3 - 50 3333 - 200
Far Infrared FIR 50 - 1000 200 - 10

Wavenumber = Frequency/wavelength

o Fourier Transform Infra Red spectroscopy (FTIR) was developed in

the early 1970s.
o Offered a number of advantages over conventional infrared
systems, including sensitivity, speed and improved data processing
,
Molecular transitions Vibrational-rotational transition

v = vib. QN
J = rot. QN
Basic components and working of FTIR

A typical interferogram
 SAMPLE PREPARATION FOR FTIR

Sampling of solids
a) Mull technique: The finely crushed sample is mixed with Nujol (
mulling agent). A thin film is applied onto the salt plates. This is then mo
unted and the spectrum is recorded
b) Solid run in Solution – Solid sample may be dissolved in a non-aq
ueous, chemically inert solvent and the solvent is not absorbed in the ran
ge to be studied. A drop of solution is placed on the disc and solvent is ev
aporated to dryness
c) Case film technique – If the solid is amorphous in nature then the
sample is deposited on the surface of a KBr or NaCl cell by evaporation
of a solution of the solid and ensured that the film is not too thick to pass
the radiation.
d) Pressed pellet technique – Small amount of finely ground solid sa
mple is mixed with 100 times its weight of KBr and compressed using a
hydraulic press. These pellets are transparent to IR radiation and it is use
d for analysis.
Continued…
2. Sampling of liquids
Liquid sample can be sandwiched using liquid sample cells of highly pur
ified alkali halides, normally NaCl. Other salts such as KBr and
CaF2 can also be used. Aqueous solvents cannot be used because they ca
nnot dissolve alkali halides. Organic solvents like chloroform can be use
d. The sample thickness should be selected so that the transmittance lies
between 15-20%. For most liquids, the sample cell thickness is 0.01-0.05
mm. Some salt plates are highly soluble in water, so the sample and wash
ing reagents must be anhydrous
3. Sampling of gases
The sample cell is made up of NaCl, KBr etc. and it is similar to the liqui
d sample cell. A sample cell with a long path length (5 – 10 cm) is neede
Application of FTIR

oFTIR Spectroscopy is used to analyze relevant amount of Compo

sitional and structural information
o Nature of pollutants
o Bonding mechanism
oFT-IR coupled with AAS (atomic absorption spectroscopy) is used to
assess the impact of industrial and natural activities on air quality
oIn addition to traditionnel transmission FTIR (T-FTIR) methods
modern reflectance techniques like:
o Attenuated total reflection FTIR (ATR-FTIR),
o Diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS)
are
oUsed in environmental, agricultural, pharmaceuticals, and food studies.
oThe choice of the method to be used depends on many factors such as:
the information needed (bulk versus surface analysis), the physical form
of the sample, the time required for sample preparation
Limitations of FTIR

o Significant presence of water vapour, CO2 and methane,

o The spectral regions are limited to 760-1300cm -1 , 2000-2230 c
m -1 , and 2390-3000 cm -1 .
o Not enough sensitivity is to detect very small concentrations in t
he sub-ppm level.
o Finally, spectral analysis is difficult since subtraction of
background spectra had to be carried out manually.
Thanks for paying attention