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FOURIER -TRANSFORM INFRARED
SPECTROMETER [FTIR]
06/04/16 SAGAR SAVALE 1
Content
 Introduction of Infrared Spectroscopy
 Difference between Infrared and Fourier Transform Infrared
Spectroscopy
 Introduction of FTIR
 Sample preparation
 Instrumentation
 Michelson interferometer
 Interferogram
 Advantages
 Disadvantage
 References
06/04/16 SAGAR SAVALE 2
Why Infrared Spectroscopy ?
An Infrared spectrum represents a fingerprint of a sample with
absorption peaks which correspond to the frequencies of
vibrations between the bonds of the atoms making up the
material-Because each different material is a unique combination
of atoms, no two compounds produce the exact same spectrum,
therefore IR can result in a unique identification of every different
kind of material!
FingerPrint
06/04/16 SAGAR SAVALE 3
What is Infrared?
 Infrared waves have wavelengths longer than visible but shorter than
microwaves.
 The Infrared region is divided into 3 regions :
Near IR : 0.8 to 2.5 u
Infrared region : 2.5 to 15 u
Far IR : 15u to 200 u
 Infrared radiation stimulates molecular vibrations.
 Infrared spectra are traditionally displayed as %T versus wave number.
06/04/16 SAGAR SAVALE 4
Stretching: Change in inter-atomic distance along bond axis
Bending: Change in angle between two bonds.
06/04/16 SAGAR SAVALE 5
To separate IR light, a grating is used.
Grating
Light source
Detector
Sample
Slit
To select the specified IR
light,
A slit is used.
Dispersion
Spectrometer
In order to measure an IR spectrum
the dispersion Spectrometer takes
several minutes.
Also the detector receives only
a few % of the energy of
original light source.
Fixed mirror
B.S.
Moving mirror
IR Light source
Sample
detector
An interferogram is first made
by the interferometer using IR
light.
The interferogram is calculated
and transformed
into a spectrum using a Fourier
Transform (FT).
FTIR
In order to measure an IR
spectrum,
FTIR takes only a few seconds.
Moreover, the detector receives
up to 50% of the energy of
original light source.
(much larger than the dispersion
spectrometer) .
06/04/16 SAGAR SAVALE 6
• Difference between FTIR and dispersive IR:
Sr.no. Dispersive IR Fourier Transform IR
1 There are many moving parts resulting in
mechanical slippage and wear. Only the mirror moves during an experiment
2 Calibration against reference spectra is
required to measure frequency .
Use of a laser provides high frequency (to 0.01
cm-1).
3 Slow scanning speed. Rapid scan speeds permit monitoring sample
undergoing rapid change.
4 In order to improve resolution only a small
amount of the IR beam may be allowed to
pass through the slits.
A much larger beam may be used at all times.
Data collection is easier .
5 Only radiation of a narrow frequency range
falls on the detector at any one time .
All frequencies of radiation fall on the detector
simultaniously .
6 The samples is subject to thermal effect
from the focused beam .
The sample is not subject to thermal effects.
7 Less sensitive, time consuming. High sensitivity ,precision & faster .
06/04/16 SAGAR SAVALE 7
FTIR
 FTIR is a powerful tool for identifying the type of chemical bond present in
a molecule.
 FTIR have greatly extended the capabilities of IR and applied to many areas
that are difficult to analyze by dispersive instrument.
 In dispersive IR , IR light is separated into it’s individual frequency by
dispersion using a grating monochromatic
 All frequencies and intensities can be simultaneously determined.
FTIR gives a plot of intensity v/s frequency.
 The instrument used for FTIR is Scanning Michelson interferometer.
 FTIR frequencies are allowed to intersect to produce an interference pattern
and this pattern is analyzed mathematically using “FOURIER
TRANSFORM”, to determine the individual frequencies and their
intensities.
06/04/16 SAGAR SAVALE 8
FTIR Instrumentation
The Michelson interferometer consist of following parts:
1) A moving mirror.
2) A fixed mirror.
3) A beam splitter.
4) A radiation source.
5) FTIR Detector.
06/04/16 SAGAR SAVALE 9
FTIR Instrumentation
06/04/16 SAGAR SAVALE 10
Sample Preparation
06/04/16 SAGAR SAVALE 11
•To obtain an spectrum, the sample must be
placed in a “container” or cell that is transparent
in the IR region of the spectrum.
•Sodium chloride or salt plates are a common
means of placing the sample in the light beam of
the instrument.
Sample Cell
06/04/16 SAGAR SAVALE 12
06/04/16 SAGAR SAVALE 13
Sources
Nernst Glower
Hollow rod about 2mm in diameter & 30 mm in length,composed
of rare earth oxide.
Externally heated (1000-1800 C).
Radiation over wide wavelength range.
Globar source
Rod of sintered silicon carbide,50mm in length & 4-8mm in diameter,
Self starting.
Heated to temp.between 1300-1700 C.
06/04/16 SAGAR SAVALE 14
Tungsten Incandescent Lamp
Black body source
Used in near IR instrument.
Nichrome/Rhodium wire
Coiled , heated
Emits in Mid-IR
Black oxide layer formation.
06/04/16 SAGAR SAVALE 15
FTIR DETECTOR
A)Thermal Detector
1) Thermocouple-
Two junctions of dissimilar metals connected together.
Electricity directly propotional to energy difference between 2
connections.
2)Bolometer-
One arm of Wheastone bridge & similar strip of metal is used as balancing
arm of bridge which is not expose to radiation.
Amount of current flowing is directly prop. to amount of radiation falling
on the detector.
06/04/16 SAGAR SAVALE 16
B)Photon detector
Interaction between incident photon and semiconductor.
Energy from photon stricking electron in detector and raises them
from non-conducting to conductance state.
E.g. MCT detector.
C) Pyroelectric Detector
DTGS Detector
06/04/16 SAGAR SAVALE 17
Interferogram
The Interferogram consist of two modulated waves :
1) Consructive Interference.
2) Destructive Interference.
λλλλλλλλλλλλλλλλλλλλλλλλλ=++++λλλ
06/04/16 SAGAR SAVALE 18
δ = nλ Constructive Interference will take place for any value of δ
when the two beams are in phase
n=0,1,2,3,…..
06/04/16 SAGAR SAVALE 19
Destructive Interference
Fixed Mirror
Moving Mirror
δ = ( n + 1/2 ) λ Totally destructive interference takes place when optical path
difference is 1/2 λ or some multiple of it-beams are completely out of phase
06/04/16 SAGAR SAVALE 20
Advantages
• Fellgette advantage- High speed.
• Jacquinot advantage-High sensitivity.
• Slitless system.
• All of the energy of the source is utilized in FTIR.
• Rapid scan time with high sensitivity.
• Connes advantage.
06/04/16 SAGAR SAVALE 21
Disadvantages
FTIR instruments have a single beam, whereas dispersive
instruments usually have a double beam.
Interferograms are difficult to interpret without first
performing a Fouriertransform to produce a spectrum.
06/04/16 SAGAR SAVALE 22
References
William Kemp, Organic Spectroscopy, Published by Palgrave,
Third edition.
Gurdeep R.Chatwal, Sham K.Anand,Instrumental method of
Chemical analysis, Himalaya Publishing house,fifth edition.
Silverstein, A Spectroscopic Identification of Organic
compound,sixth edition.
Skoog wele Hollers, Analytical chemistry Introduction ,
Saunderls college publishing house ,eight edition.
B.K Sharma, Instrumental method of chemical analysis, Goel
publication, second edition.
Y.R Sharma, Elementary Organic Spectroscopy,Principles and
Chemical applications, S.Chand Publication, sixth edition.
06/04/16 SAGAR SAVALE 23
HabartH .Willard,Lynne L. Merritt,Johan A. Dean,
Frank A.Settle,Instrumental method of Analysis, CBS
Publisher and Distributors, New Delhi.
Dyer R John, Application of Absorption Spectroscopy
of unknown Organic compound, PHT, pvt. Ltd. New
Delhi.
06/04/16 SAGAR SAVALE 24
06/04/16 SAGAR SAVALE 25

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FOURIER -TRANSFORM INFRARED SPECTROMETER [FTIR]

  • 1. FOURIER -TRANSFORM INFRARED SPECTROMETER [FTIR] 06/04/16 SAGAR SAVALE 1
  • 2. Content  Introduction of Infrared Spectroscopy  Difference between Infrared and Fourier Transform Infrared Spectroscopy  Introduction of FTIR  Sample preparation  Instrumentation  Michelson interferometer  Interferogram  Advantages  Disadvantage  References 06/04/16 SAGAR SAVALE 2
  • 3. Why Infrared Spectroscopy ? An Infrared spectrum represents a fingerprint of a sample with absorption peaks which correspond to the frequencies of vibrations between the bonds of the atoms making up the material-Because each different material is a unique combination of atoms, no two compounds produce the exact same spectrum, therefore IR can result in a unique identification of every different kind of material! FingerPrint 06/04/16 SAGAR SAVALE 3
  • 4. What is Infrared?  Infrared waves have wavelengths longer than visible but shorter than microwaves.  The Infrared region is divided into 3 regions : Near IR : 0.8 to 2.5 u Infrared region : 2.5 to 15 u Far IR : 15u to 200 u  Infrared radiation stimulates molecular vibrations.  Infrared spectra are traditionally displayed as %T versus wave number. 06/04/16 SAGAR SAVALE 4
  • 5. Stretching: Change in inter-atomic distance along bond axis Bending: Change in angle between two bonds. 06/04/16 SAGAR SAVALE 5
  • 6. To separate IR light, a grating is used. Grating Light source Detector Sample Slit To select the specified IR light, A slit is used. Dispersion Spectrometer In order to measure an IR spectrum the dispersion Spectrometer takes several minutes. Also the detector receives only a few % of the energy of original light source. Fixed mirror B.S. Moving mirror IR Light source Sample detector An interferogram is first made by the interferometer using IR light. The interferogram is calculated and transformed into a spectrum using a Fourier Transform (FT). FTIR In order to measure an IR spectrum, FTIR takes only a few seconds. Moreover, the detector receives up to 50% of the energy of original light source. (much larger than the dispersion spectrometer) . 06/04/16 SAGAR SAVALE 6
  • 7. • Difference between FTIR and dispersive IR: Sr.no. Dispersive IR Fourier Transform IR 1 There are many moving parts resulting in mechanical slippage and wear. Only the mirror moves during an experiment 2 Calibration against reference spectra is required to measure frequency . Use of a laser provides high frequency (to 0.01 cm-1). 3 Slow scanning speed. Rapid scan speeds permit monitoring sample undergoing rapid change. 4 In order to improve resolution only a small amount of the IR beam may be allowed to pass through the slits. A much larger beam may be used at all times. Data collection is easier . 5 Only radiation of a narrow frequency range falls on the detector at any one time . All frequencies of radiation fall on the detector simultaniously . 6 The samples is subject to thermal effect from the focused beam . The sample is not subject to thermal effects. 7 Less sensitive, time consuming. High sensitivity ,precision & faster . 06/04/16 SAGAR SAVALE 7
  • 8. FTIR  FTIR is a powerful tool for identifying the type of chemical bond present in a molecule.  FTIR have greatly extended the capabilities of IR and applied to many areas that are difficult to analyze by dispersive instrument.  In dispersive IR , IR light is separated into it’s individual frequency by dispersion using a grating monochromatic  All frequencies and intensities can be simultaneously determined. FTIR gives a plot of intensity v/s frequency.  The instrument used for FTIR is Scanning Michelson interferometer.  FTIR frequencies are allowed to intersect to produce an interference pattern and this pattern is analyzed mathematically using “FOURIER TRANSFORM”, to determine the individual frequencies and their intensities. 06/04/16 SAGAR SAVALE 8
  • 9. FTIR Instrumentation The Michelson interferometer consist of following parts: 1) A moving mirror. 2) A fixed mirror. 3) A beam splitter. 4) A radiation source. 5) FTIR Detector. 06/04/16 SAGAR SAVALE 9
  • 12. •To obtain an spectrum, the sample must be placed in a “container” or cell that is transparent in the IR region of the spectrum. •Sodium chloride or salt plates are a common means of placing the sample in the light beam of the instrument. Sample Cell 06/04/16 SAGAR SAVALE 12
  • 14. Sources Nernst Glower Hollow rod about 2mm in diameter & 30 mm in length,composed of rare earth oxide. Externally heated (1000-1800 C). Radiation over wide wavelength range. Globar source Rod of sintered silicon carbide,50mm in length & 4-8mm in diameter, Self starting. Heated to temp.between 1300-1700 C. 06/04/16 SAGAR SAVALE 14
  • 15. Tungsten Incandescent Lamp Black body source Used in near IR instrument. Nichrome/Rhodium wire Coiled , heated Emits in Mid-IR Black oxide layer formation. 06/04/16 SAGAR SAVALE 15
  • 16. FTIR DETECTOR A)Thermal Detector 1) Thermocouple- Two junctions of dissimilar metals connected together. Electricity directly propotional to energy difference between 2 connections. 2)Bolometer- One arm of Wheastone bridge & similar strip of metal is used as balancing arm of bridge which is not expose to radiation. Amount of current flowing is directly prop. to amount of radiation falling on the detector. 06/04/16 SAGAR SAVALE 16
  • 17. B)Photon detector Interaction between incident photon and semiconductor. Energy from photon stricking electron in detector and raises them from non-conducting to conductance state. E.g. MCT detector. C) Pyroelectric Detector DTGS Detector 06/04/16 SAGAR SAVALE 17
  • 18. Interferogram The Interferogram consist of two modulated waves : 1) Consructive Interference. 2) Destructive Interference. λλλλλλλλλλλλλλλλλλλλλλλλλ=++++λλλ 06/04/16 SAGAR SAVALE 18
  • 19. δ = nλ Constructive Interference will take place for any value of δ when the two beams are in phase n=0,1,2,3,….. 06/04/16 SAGAR SAVALE 19
  • 20. Destructive Interference Fixed Mirror Moving Mirror δ = ( n + 1/2 ) λ Totally destructive interference takes place when optical path difference is 1/2 λ or some multiple of it-beams are completely out of phase 06/04/16 SAGAR SAVALE 20
  • 21. Advantages • Fellgette advantage- High speed. • Jacquinot advantage-High sensitivity. • Slitless system. • All of the energy of the source is utilized in FTIR. • Rapid scan time with high sensitivity. • Connes advantage. 06/04/16 SAGAR SAVALE 21
  • 22. Disadvantages FTIR instruments have a single beam, whereas dispersive instruments usually have a double beam. Interferograms are difficult to interpret without first performing a Fouriertransform to produce a spectrum. 06/04/16 SAGAR SAVALE 22
  • 23. References William Kemp, Organic Spectroscopy, Published by Palgrave, Third edition. Gurdeep R.Chatwal, Sham K.Anand,Instrumental method of Chemical analysis, Himalaya Publishing house,fifth edition. Silverstein, A Spectroscopic Identification of Organic compound,sixth edition. Skoog wele Hollers, Analytical chemistry Introduction , Saunderls college publishing house ,eight edition. B.K Sharma, Instrumental method of chemical analysis, Goel publication, second edition. Y.R Sharma, Elementary Organic Spectroscopy,Principles and Chemical applications, S.Chand Publication, sixth edition. 06/04/16 SAGAR SAVALE 23
  • 24. HabartH .Willard,Lynne L. Merritt,Johan A. Dean, Frank A.Settle,Instrumental method of Analysis, CBS Publisher and Distributors, New Delhi. Dyer R John, Application of Absorption Spectroscopy of unknown Organic compound, PHT, pvt. Ltd. New Delhi. 06/04/16 SAGAR SAVALE 24