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IR SPECTROSCOPY
By:-
Vishal Singh
B.Tech(Biotech) 3rd Year
I.E.T,B.U
Jhansi
Spectroscopy is the science which study
the interaction between the radiation
and matter
Historically, spectroscopy originated
through the study of visible light
dispersed according to its wavelength,
by a prism
Some Spectroscopy Types:-
 Ultraviolet and Visible Spectoscopy
 Fluorescence spectroscopy
 Infrared and Raman Spectroscopy
 X-ray Diffraction
 Atomic Spectroscopy
 Circular dichroism Spectroscopy
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 Spectoscopy:-
 A method of obtaining an Infrared spectrum by measuring the
interferogram of a sample using an interferometer, then
performing a Fourier Transform upon the interferogram to obtain
the spectrum.
 .
Principle:-
• FTIR relies on the fact that the most molecules absorb light in the
infra-red region of the electromagnetic spectrum.
• This absorption corresponds specifically to the bonds present in
the molecule. The frequency range are measured as wave
numbers typically over the range 4000 – 600 cm-1.
• The background emission spectrum of the IR source is first
recorded, followed by the emission spectrum of the IR source
with the sample in place.
• The ratio of the sample spectrum to the background spectrum
is directly related to the sample's absorption spectrum.
• The resultant absorption spectrum from the bond natural
vibration frequencies indicates the presence of various
chemical bonds and functional groups present in the sample.
• FTIR is particularly useful for identification of organic
molecular groups and compounds due to the range of
functional groups, side chains and cross-links involved, all of
which will have characteristic vibrational frequencies in the
infra-red range.
Interferometer:-
• To make an interferogram, we combine light from two
different sources. In practice, we use the same light source (a
laser ) and split the light into two beams.
• One is the reference beam, which will provide a comparison
wavefront. The other is the test beam , which is passed
through the optical system to be tested. The two beams are
combined together to make an interferogram
• Most interferometers employ a beamsplitter which takes
the incoming infrared beam and divides it into two optical
beams.
• One beam reflects off of a flat mirror which is fixed in place.
The other beam reflects off of a flat mirror which is on a
mechanism which allows this mirror to move a very short
distance (typically a few millimeters) away from the
beamsplitter.
• The two beams reflect off of their respective mirrors and are
recombined when they meet back at the beamsplitter.
Because the path that one beam travels is a fixed length and
the other is constantly changing as its mirror moves, the
signal which exits the interferometer is the result of these
two beams “interfering” with each other.
• The resulting signal is called an interferogram which has the
unique property that every data point (a function of the
moving mirror position) which makes up the signal has
information about every infrared frequency
Sampling Techniques:-
1.Liquid Samples:
Neat sample
Diluted solution
Liquid cell
2.Solid Samples:
Neat sample
Cast films
Pressed films
KBr pellets
Mull
3.Gas Samples:
Short path cell
Long path cell
Intrumentation:-
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” takesplace. 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.
Dispersive IR Fourier transform IR
1. There are many moving parts,
resulting in mechanical slippage.
2. Calibration against reference spectra
is required to measure frequency.
3. Stray light causes spurious readings.
4. To improve resolution only a small
amount of IR beam is allowed to pass.
1. Only the mirror moves during the
experiment.
2. Use of laser provides high frequency
accuracy (to 0.01 cm-1).
3. Stray radiations do not affect the
detector.
4. A much larger beam may be used at
all time. Data collection is easier.
Applications of FTIR:-
• Identification of simple mixtures of organic and inorganic compounds both as
solids or liquids.
• Identification of polymers and polymer blends.
• Indirect verification of trace organic contaminants on surfaces
• Analysis of Analysis of adhesives, coatings and adhesion promoters or coupling agents.
• Small visible particle chemical analysis..
• Identification of rubbers and filled rubbers.
• Determination of degrees of crystallinity in polymers (eg LDPE and HDPE).
• Compararive chain lengths in organics.
• Extent of thermal, UV or other degredation or depolymerisation of polymers and paint
coatings.
• Analysis of a gaseous samples using a gas cell for headspace analysis or environmental
monitoring.
• Analysis of unknown solvents, cleaning agents and detergents.
References:-
1. Principles and Techniques of Biochemistry and Molecular Biology
-Keith Wilson And John Walker
2. Introduction to Spectroscopy
-Donald A. Pavia
3. http://www.lpdlabservices.co.uk/
4. //en.wikipedia.org
Ftir

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Ftir

  • 2. Spectroscopy is the science which study the interaction between the radiation and matter Historically, spectroscopy originated through the study of visible light dispersed according to its wavelength, by a prism
  • 3.
  • 4. Some Spectroscopy Types:-  Ultraviolet and Visible Spectoscopy  Fluorescence spectroscopy  Infrared and Raman Spectroscopy  X-ray Diffraction  Atomic Spectroscopy  Circular dichroism Spectroscopy
  • 5. 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.
  • 6. FTIR Spectoscopy:-  A method of obtaining an Infrared spectrum by measuring the interferogram of a sample using an interferometer, then performing a Fourier Transform upon the interferogram to obtain the spectrum.  .
  • 7. Principle:- • FTIR relies on the fact that the most molecules absorb light in the infra-red region of the electromagnetic spectrum. • This absorption corresponds specifically to the bonds present in the molecule. The frequency range are measured as wave numbers typically over the range 4000 – 600 cm-1. • The background emission spectrum of the IR source is first recorded, followed by the emission spectrum of the IR source with the sample in place.
  • 8. • The ratio of the sample spectrum to the background spectrum is directly related to the sample's absorption spectrum. • The resultant absorption spectrum from the bond natural vibration frequencies indicates the presence of various chemical bonds and functional groups present in the sample. • FTIR is particularly useful for identification of organic molecular groups and compounds due to the range of functional groups, side chains and cross-links involved, all of which will have characteristic vibrational frequencies in the infra-red range.
  • 10. • To make an interferogram, we combine light from two different sources. In practice, we use the same light source (a laser ) and split the light into two beams. • One is the reference beam, which will provide a comparison wavefront. The other is the test beam , which is passed through the optical system to be tested. The two beams are combined together to make an interferogram • Most interferometers employ a beamsplitter which takes the incoming infrared beam and divides it into two optical beams.
  • 11. • One beam reflects off of a flat mirror which is fixed in place. The other beam reflects off of a flat mirror which is on a mechanism which allows this mirror to move a very short distance (typically a few millimeters) away from the beamsplitter. • The two beams reflect off of their respective mirrors and are recombined when they meet back at the beamsplitter. Because the path that one beam travels is a fixed length and the other is constantly changing as its mirror moves, the signal which exits the interferometer is the result of these two beams “interfering” with each other. • The resulting signal is called an interferogram which has the unique property that every data point (a function of the moving mirror position) which makes up the signal has information about every infrared frequency
  • 12. Sampling Techniques:- 1.Liquid Samples: Neat sample Diluted solution Liquid cell 2.Solid Samples: Neat sample Cast films Pressed films KBr pellets Mull 3.Gas Samples: Short path cell Long path cell
  • 14. 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” takesplace. The resulting interferogram signal then exits the interferometer.
  • 15. 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.
  • 16. Dispersive IR Fourier transform IR 1. There are many moving parts, resulting in mechanical slippage. 2. Calibration against reference spectra is required to measure frequency. 3. Stray light causes spurious readings. 4. To improve resolution only a small amount of IR beam is allowed to pass. 1. Only the mirror moves during the experiment. 2. Use of laser provides high frequency accuracy (to 0.01 cm-1). 3. Stray radiations do not affect the detector. 4. A much larger beam may be used at all time. Data collection is easier.
  • 17. Applications of FTIR:- • Identification of simple mixtures of organic and inorganic compounds both as solids or liquids. • Identification of polymers and polymer blends. • Indirect verification of trace organic contaminants on surfaces • Analysis of Analysis of adhesives, coatings and adhesion promoters or coupling agents. • Small visible particle chemical analysis.. • Identification of rubbers and filled rubbers. • Determination of degrees of crystallinity in polymers (eg LDPE and HDPE). • Compararive chain lengths in organics. • Extent of thermal, UV or other degredation or depolymerisation of polymers and paint coatings. • Analysis of a gaseous samples using a gas cell for headspace analysis or environmental monitoring. • Analysis of unknown solvents, cleaning agents and detergents.
  • 18. References:- 1. Principles and Techniques of Biochemistry and Molecular Biology -Keith Wilson And John Walker 2. Introduction to Spectroscopy -Donald A. Pavia 3. http://www.lpdlabservices.co.uk/ 4. //en.wikipedia.org