FTIR PRESENTATION

INTROUDCTION
• FT-IR stands for Fourier Transform InfraRed, the preferred method of
infrared spectroscopy.
• In infrared spectroscopy, IR radiation is passed through a sample.
• Some of the infrared radiation is absorbed by the sample and some of it
is passed through (transmitted).
• The resulting spectrum represents the molecular absorption and
transmission, creating a molecular fingerprint of the sample.
• Like a fingerprint no two unique molecular structures produce the same
infrared spectrum.
• This makes infrared spectroscopy useful for several types of analysis
• FTIR method is a method of exploring the physical properties of solids,
liquids, and gases.
• More specifically, it allows the study of the absorptive and emissive
properties of materials.
• The choice of IR wavelengths in FTIR method is particularly useful for
studying chemical bonds that connect atoms.
• It turns out that these bonds tend to vibrate with frequencies that
correspond to infrared-wavelength light, and hence can easily be excited
with such a radiation.
• Commonly, IR wavelength spectroscopy covers wavenumbers ranging from
200 to 4000 cm^-1
principles
• The most important component of FTIR spectroscopy, and where it
derives its distinction from typical infrared spectroscopy, is the
Michelson interferometer.
• Whereas in dispersive IR spectroscopy monochromatic light
sequentially irradiates a sample spanning an infrared wavelength
range, FTIR spectroscopy irradiates a sample with many frequencies
of IR light at once, utilizing an interferometer and post-processing of
the transmitted light.
Principles
• A beam source of various IR wavelength light is sent through a beam splitter,
where half reaches a fixed mirror and half a mirror that moves with a
constant velocity.
• These two split beams are then reflected and recombined (now with a path
difference between the beams) to construct an interference pattern
reflecting the constructive and destructive interference of the recombination.
• After, this interference pattern (or interferogram) is sent to the sample, and
the transmitted portion of the interferogram is sent to a detector.
• After comparison with a reference sample beam spectrum in the detector, a
Fourier transform is performed to obtain the full spectrum as a function of
wavenumber.
principles
• While all of this might seem quite arcane when compared to the seemingly
simple technique of sequential monochromatic irradiation, Fourier-transform
spectroscopy offers a number of key benefits that have made it the dominant
method of IR spectroscopy.
• When information from all wavelengths is collected at once, there tends to be
signal-to-noise ratio reduction in the output spectra.
• Furthermore, the more obvious benefit of performing all wavelength
measurements at once is the speed reduction when compared to dispersive
wavelength techniques.
• However, since FTIR has been unquestioned industry standard for many
decades now, it is possible that forthcoming technique breakthroughs or
advances in dispersive techniques may yet catch up.
FTIR: What is it Good For?
• Since just about all materials are able to be analyzed by FTIR
spectroscopy to provide valuable information, but it has perhaps
found its most frequent use in the analysis of carbon-containing
organic compounds, for which there is a comprehensive knowledge
base of characteristic vibrational frequencies.
• As previously mentioned, chemical bonds between atoms vibrate at
characteristic frequencies which have been widely tabulated, allowing
for determination of the composition of samples or presence of
potential contaminants by comparing the peaks of an IR spectra with
tabulated characteristic frequencies.
FTIR: What is it Good For?
• Furthermore, quality analysis of various samples can also be
determined using FTIR.
• For example, deviations in the characteristic spectra from a material
can be indicators of oxidation or other contamination.
• In polymers, deviations from an expected IR spectrum can indicate a
different degree of polymerization (curing) or decomposition from a
reference sample.
• For these reasons, FTIR is widely used in such disparate applications
as polymer characterization, forensic analysis, pharmaceutical
analysis, and food testing.
The normal instrumental process is as follows

• : 1. The Source: Infrared energy is emitted from a glowing black-body source. This beam passes
through an aperture which controls the amount of energy presented to the sample (and, ultimately, to
the detector).
• 2. The Interferometer: The beam enters the interferometer where the “spectral encoding” takes place.
The resulting interferogram signal then exits the interferometer.
• 3. The Sample: The beam enters the sample compartment where it is transmitted through or reflected
off of the surface of the sample, depending on the type of analysis being accomplished. This is where
specific frequencies of energy, which are uniquely characteristic of the sample, are absorbed.
• 4. The Detector: The beam finally passes to the detector for final measurement. The detectors used are
specially designed to measure the special interferogram signal.
• 5. The Computer: The measured signal is digitized and sent to the computer where the Fourier
transformation takes place.
• The final infrared spectrum is then presented to the user for interpretation and any further
manipulation
Schematic diagram showing the
working principle of an
interferometer.
The sample analysis process
• Because there needs to be a relative scale for the absorption intensity, a
background spectrum must also be measured.
• This is normally a measurement with no sample in the beam.
• This can be compared to the measurement with the sample in the beam to
determine the “percent transmittance.”
• This technique results in a spectrum which has all of the instrumental
characteristics removed.
• Thus, all spectral features which are present are strictly due to the sample.
• A single background measurement can be used for many sample
measurements because this spectrum is characteristic of the instrument itself
Interpreting the IR spectrum
• The graph produced show percentage transmission against wave number
• If no radiation is absorbed at a particular frequency, then the line on the graph will be at
100% at the corresponding wave number
• Identification possible due to differences in the chemical structure of materials
characteristic vibration and yield unique IR spectra (fingerprint)
• Different types of bonds have characteristic regions of the spectrum where they absorb
Most functional groups absorb above 1500 cm-1.
• The region below 1500 cm-1 is known as the "fingerprint region".
• Every molecule produces a unique pattern here, so if an unknown sample produces a
spectrum which matches that of a known compound, the sample can be confirmed to be
that compound
• Chart showing the IR bands produced by the major functional groups and
the fingerprint region specific to each compoun
Interpreting the IR spectrum
SAMPLE PREPARATION
• If the sample is a liquid, it can be tested straight away.
• If it is a solid, it is prepared by grinding the sample with KBr and
compressing the whole into a transparent disk.
• KBr must be dry in order to avoid formation of broad absorptions due
to moisture.
• A thin layer of the liquid or finely ground solid is placed in the sample
holder and placed in the machine.
ADVANTAGES
• Speed: because all the frequencies are measured simultaneously, most
measurements are made in a matter of seconds than several minutes.
• Sensitivity : detectors used are more, the optical throughput is much higher
which results in much lower noise levels.
• Mechanical simplicity: the moving mirror in the interferometer is the only
continuously moving part in the instrument.
• Thus there is very little possibility of mechanical breakdown.
• Internally calibrated: these instruments employ a HeNe laser as an internal
wavelength calibration standard .
• These instruments are self calibrating and never need to be calibrated by the
user.
LIMITATIONS
• Material with similar structures are very difficult to differentiate
• The analysis is highly dependent upon libraries
• Complex mixtures can be difficult to properly analyse
• Quantitative analysis of components or contaminates in a material is
difficult
• Detection limit are generally 1%-5%
APPLICATIONS
• Identification of functional groups and structure-elucidation of
organic compounds
• quantitative analysis of a number of organic compounds
• -detection of impurites in a compound
• -study the presence of water in a sample
• -ratio of cus-trans isomers in a mixture of compounds
• -studying the progress of reactions