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IR and FT-IR
Presented By,
Chetan M. Jain
First Year M.Pharm
(Quality Assurance)
Government College of Pharmacy,Amravati.
11/12/16
InFRaRed
SpecTRoScopy
 Intoroduction
2
Provide useful information about structure of molecule.
Absorption of IR radiation by molecule and exhibit absorption
spectra.
Change in dipole moment.
Energy of radiation is directly proportional to wave number and
inversely proportional to wavelength.
Region Wavelength (µ) Wave number (cm-1
)
Near IR 0.75-2.5 1200-4000
Infrared 2.5-16 4000-625
Far IR 16-200 625-10 11/12/16
Chetan Jain
oRIgIn oF IR SpecTRa
 UV- Visible spectrum results in changes of electronic as
well as vibrational and rotational level in molecule.
 IR radiation shows only vibrational and rotational level.
 Vibrational-Rotational spectrum.
3 11/12/16Chetan Jain
4
11/12/16Chetan Jain
InSTRumenTaTIon
The optical components of IR spectrophotometer are
5
Light Source
Monochromator
Sample Holder
Detector
Recorder
11/12/16Chetan Jain
Dispersive instruments
FT-IR instrument
Non-dispersive instruments
IR RadIaTIon SouRce
 Hot bodies continuously emmitting radiation
 Incandescent lamp
 Nernst Glover
6
A closed wound nichrome wire is used.
A black oxide film formed on the coil gives emissivity by heating.
Temp. can be raised to 1100°C.
Used in near IR region and failed in IR region.
In IR region – most common source.
Consists of hollow rod-2mm in dia and 2-5cm in length.
Composed of mixture of oxides like zirconium, yttrium and thorium.
Temp: 1000-1800°C.
11/12/16Chetan Jain
 Advantages of Nernst glower
 Disadvantage
7
It emits IR radiation over wide range of wavelength.
The intensity of radiation maintains steady and constant over long period
of time.
Used in air as it is not oxidized.
Frequent mechanical failure.
11/12/16Chetan Jain
 Globar Source
 Mercury Arc
 Tungsten Filament lamp
8
It is rod of sintered silicon carbide about 5cm in length and 4mm in
diameter
Temp- 1300°C.
 If radiation above 10µ it is used.
Far IR region it is used.
It is encolosed in quartz jacket to reduce loss.
Useful for near IR region only.
11/12/16Chetan Jain
MonochroMators
 Select desired frequencies and reject other frequencies.
 These are of two types
9
1) Prism Monochromator
2) Grating Monochromator
11/12/16Chetan Jain
PrisM
MonochroMator
 Greater range and simplicity.
 Halogens salts are used.
 Crystalline NaCl: 5-15µ
 Crystalline KBr/CBr: 15-40 µ
 LiF : 0.75-2.5
 Two types
10
Single beam monochromator
Double beam Monochromator
11/12/16Chetan Jain
GratinG MonochroMator
 Series of parallel straight lines cut into plane
surface.
 Constructed from glass coated with aluminium.
 Gives radiation into single order.
 Advantages
11
Not attacked by moisture.
Used over considerable wavelength.
Sturdy and long lasting.
11/12/16Chetan Jain
saMPle holders and saMPlin
of substance
 Used for solid, liquid and gas.
 Material containing sample must be transperent to
IR region.
 Sample cell constructed from rock salt.
 Sample must be pure and free from water.
12 11/12/16Chetan Jain
saMPlinG of solids
 Solid dissolved in solvent
 As Solid Film
 Mull technique
13
Carbon tetrachloride,Chloroform,acetone and cyclohexane.
Sample solution is placed on surface of KBr or Nacl and
allowed to evaporate.
Solid sample mixed with nujol to form a paste. This paste is
then sandwiched between two salt plates and used for spectral
measurement.
Nujol has absorption at 2915,1462,1376 and 719cm-1
11/12/16Chetan Jain
 Pressed Pellet Technique(Disk Method)
 Advatages of pellet tech. over mull tech. is
14
The small amount of finally ground solid sample is mixed with
100 times its weight of powdered KBr.
This mixture is pressed under high pressure in IR tablet press
to form pellet.
Eliminates the problem of band
If KBr pellet is preserved can be reused
Resolution of KBr is superior
11/12/16Chetan Jain
saMPlinG of liquids
 For sampling of various cell like sandwitch cell,demountable cell
and cavity cell are used.
 Made up of Nacl, KBr or thallium bromide.
 Demountable cell:
 Cavity cell:
15
It consists of pair of salt plates separeted by gasket made of
metal or teflon and together by an clamp.
Matching a parallel-sided hole in a salt block makes it.
11/12/16Chetan Jain
saMPlinG of Gas
 The dried gases introduced via a stop cock.
 The gas sample is introduced into the gas cell made up of
glass or metal cylinder of about 10cm long.
 The end walls of the gas cell made up of NaCl.
16 11/12/16Chetan Jain
Detectors
 Two types of detectors are used
 Thermal detectors
17
Thermal detectors
Photodetectors
When IR radiation falls on these detectors they cause heating
which give rise to P.D. This P.D. is depends upon amt of
radiation. Thermocouple
Bolometer
Thermister
Golay cell 11/12/16Chetan Jain
 Thermocouple
18
These are dissimilar strips of metal join together at one end.
Two fine wires of metals are welded with blackened gold foil,
which absorbs radiation.
One welded joint(Cold junction) is kept at constant temp.
The other welded joint (Hot junction) is exposed to radiation.
This exposure of hot junction causes rise in its temp, cause the
P.D. proportional to the amt of radiation.
11/12/16Chetan Jain
 Bolometers
19
These are constructed from metals or semiconductors.
When IR radiation falls on bolometer its temp. changes cause
change in the resistence of the conductor.
This change in the resistence of conductor is depends upon amt
of radiation.
This made one arm of Wheistone Bridge.
If IR radiation falls on the bolometer, the bridge becomes
unbalanced due to change in the electrical resistence causes
current flow through galvanometer.this amt of current flow is a
measure of intensity of radiation.
11/12/16Chetan Jain
 Thermister
20
These function similar to bolometer.
These are the resisters made by fusing several metallic
oxides.
11/12/16Chetan Jain
 Golay cell
21
It consists of metal cylinder.
One end of which closed by balanced metal plate and other with
metalised diaphragm.
Cylinder is filled with gas like xenon.
When the radiation falls on blackened metal plate it is heated which
causes expansion of gas, which affect the motion of diaphragm.
11/12/16Chetan Jain
Photon Detectors
 Used in near IR region.
 Consists of semiconductors like lead sulphide, lead
telluride.
 When radiation are fall on these they goes to higher
level and produce signal.
 Photoconductivity cell
22
It consists of thin layer of lead sulphide supported on glass
and enclosed into an evacuated glass envelope.
11/12/16Chetan Jain
Fourier transForm ir
sPectroscoPy (Ftir)
23 11/12/16Chetan Jain
Fourier Transform IR
Spectroscopy (FTIR)
 Advanced technique.
 Interferometer(Michelson Interferometer).
24 11/12/16Chetan Jain
 Advantages
25
Fellgett Advantage
Jacquinot advantage
11/12/16Chetan Jain
InterpretatIon of Ir Spectr
26 11/12/16Chetan Jain
applIcatIonS of Ir and ft
Ir
 Qualitative application
 Quantitative application.
27 11/12/16Chetan Jain
References
 Pharamceutical analysis by A.V. Kasture, S.G. Wadodkar,K.R.
Mahadik, H.N. More, Volume II, Nirali Prakashan, Eleventh
edition (2004), p.no. 207-221.
 Fundamental of analytical chemistry by D.A.Skoog,
D.M.West,F.J.Holler,7th
edition p.no.592-597.
 Organic Spectroscopy by William Kemp, 3rd
edition, Palgrave
Publication, p.no19-56.
 Instrumental Methods of Analysis by H.A.Willard, L.L.Merritt,
J.A.Dean, F.A. Settle, 7th
edition, p.no. 288 to 320.
28 11/12/16Chetan Jain
29 11/12/16Chetan Jain

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IR and FT-IR Spectroscopy Explained

  • 1. 1 IR and FT-IR Presented By, Chetan M. Jain First Year M.Pharm (Quality Assurance) Government College of Pharmacy,Amravati. 11/12/16
  • 2. InFRaRed SpecTRoScopy  Intoroduction 2 Provide useful information about structure of molecule. Absorption of IR radiation by molecule and exhibit absorption spectra. Change in dipole moment. Energy of radiation is directly proportional to wave number and inversely proportional to wavelength. Region Wavelength (µ) Wave number (cm-1 ) Near IR 0.75-2.5 1200-4000 Infrared 2.5-16 4000-625 Far IR 16-200 625-10 11/12/16 Chetan Jain
  • 3. oRIgIn oF IR SpecTRa  UV- Visible spectrum results in changes of electronic as well as vibrational and rotational level in molecule.  IR radiation shows only vibrational and rotational level.  Vibrational-Rotational spectrum. 3 11/12/16Chetan Jain
  • 5. InSTRumenTaTIon The optical components of IR spectrophotometer are 5 Light Source Monochromator Sample Holder Detector Recorder 11/12/16Chetan Jain Dispersive instruments FT-IR instrument Non-dispersive instruments
  • 6. IR RadIaTIon SouRce  Hot bodies continuously emmitting radiation  Incandescent lamp  Nernst Glover 6 A closed wound nichrome wire is used. A black oxide film formed on the coil gives emissivity by heating. Temp. can be raised to 1100°C. Used in near IR region and failed in IR region. In IR region – most common source. Consists of hollow rod-2mm in dia and 2-5cm in length. Composed of mixture of oxides like zirconium, yttrium and thorium. Temp: 1000-1800°C. 11/12/16Chetan Jain
  • 7.  Advantages of Nernst glower  Disadvantage 7 It emits IR radiation over wide range of wavelength. The intensity of radiation maintains steady and constant over long period of time. Used in air as it is not oxidized. Frequent mechanical failure. 11/12/16Chetan Jain
  • 8.  Globar Source  Mercury Arc  Tungsten Filament lamp 8 It is rod of sintered silicon carbide about 5cm in length and 4mm in diameter Temp- 1300°C.  If radiation above 10µ it is used. Far IR region it is used. It is encolosed in quartz jacket to reduce loss. Useful for near IR region only. 11/12/16Chetan Jain
  • 9. MonochroMators  Select desired frequencies and reject other frequencies.  These are of two types 9 1) Prism Monochromator 2) Grating Monochromator 11/12/16Chetan Jain
  • 10. PrisM MonochroMator  Greater range and simplicity.  Halogens salts are used.  Crystalline NaCl: 5-15µ  Crystalline KBr/CBr: 15-40 µ  LiF : 0.75-2.5  Two types 10 Single beam monochromator Double beam Monochromator 11/12/16Chetan Jain
  • 11. GratinG MonochroMator  Series of parallel straight lines cut into plane surface.  Constructed from glass coated with aluminium.  Gives radiation into single order.  Advantages 11 Not attacked by moisture. Used over considerable wavelength. Sturdy and long lasting. 11/12/16Chetan Jain
  • 12. saMPle holders and saMPlin of substance  Used for solid, liquid and gas.  Material containing sample must be transperent to IR region.  Sample cell constructed from rock salt.  Sample must be pure and free from water. 12 11/12/16Chetan Jain
  • 13. saMPlinG of solids  Solid dissolved in solvent  As Solid Film  Mull technique 13 Carbon tetrachloride,Chloroform,acetone and cyclohexane. Sample solution is placed on surface of KBr or Nacl and allowed to evaporate. Solid sample mixed with nujol to form a paste. This paste is then sandwiched between two salt plates and used for spectral measurement. Nujol has absorption at 2915,1462,1376 and 719cm-1 11/12/16Chetan Jain
  • 14.  Pressed Pellet Technique(Disk Method)  Advatages of pellet tech. over mull tech. is 14 The small amount of finally ground solid sample is mixed with 100 times its weight of powdered KBr. This mixture is pressed under high pressure in IR tablet press to form pellet. Eliminates the problem of band If KBr pellet is preserved can be reused Resolution of KBr is superior 11/12/16Chetan Jain
  • 15. saMPlinG of liquids  For sampling of various cell like sandwitch cell,demountable cell and cavity cell are used.  Made up of Nacl, KBr or thallium bromide.  Demountable cell:  Cavity cell: 15 It consists of pair of salt plates separeted by gasket made of metal or teflon and together by an clamp. Matching a parallel-sided hole in a salt block makes it. 11/12/16Chetan Jain
  • 16. saMPlinG of Gas  The dried gases introduced via a stop cock.  The gas sample is introduced into the gas cell made up of glass or metal cylinder of about 10cm long.  The end walls of the gas cell made up of NaCl. 16 11/12/16Chetan Jain
  • 17. Detectors  Two types of detectors are used  Thermal detectors 17 Thermal detectors Photodetectors When IR radiation falls on these detectors they cause heating which give rise to P.D. This P.D. is depends upon amt of radiation. Thermocouple Bolometer Thermister Golay cell 11/12/16Chetan Jain
  • 18.  Thermocouple 18 These are dissimilar strips of metal join together at one end. Two fine wires of metals are welded with blackened gold foil, which absorbs radiation. One welded joint(Cold junction) is kept at constant temp. The other welded joint (Hot junction) is exposed to radiation. This exposure of hot junction causes rise in its temp, cause the P.D. proportional to the amt of radiation. 11/12/16Chetan Jain
  • 19.  Bolometers 19 These are constructed from metals or semiconductors. When IR radiation falls on bolometer its temp. changes cause change in the resistence of the conductor. This change in the resistence of conductor is depends upon amt of radiation. This made one arm of Wheistone Bridge. If IR radiation falls on the bolometer, the bridge becomes unbalanced due to change in the electrical resistence causes current flow through galvanometer.this amt of current flow is a measure of intensity of radiation. 11/12/16Chetan Jain
  • 20.  Thermister 20 These function similar to bolometer. These are the resisters made by fusing several metallic oxides. 11/12/16Chetan Jain
  • 21.  Golay cell 21 It consists of metal cylinder. One end of which closed by balanced metal plate and other with metalised diaphragm. Cylinder is filled with gas like xenon. When the radiation falls on blackened metal plate it is heated which causes expansion of gas, which affect the motion of diaphragm. 11/12/16Chetan Jain
  • 22. Photon Detectors  Used in near IR region.  Consists of semiconductors like lead sulphide, lead telluride.  When radiation are fall on these they goes to higher level and produce signal.  Photoconductivity cell 22 It consists of thin layer of lead sulphide supported on glass and enclosed into an evacuated glass envelope. 11/12/16Chetan Jain
  • 23. Fourier transForm ir sPectroscoPy (Ftir) 23 11/12/16Chetan Jain
  • 24. Fourier Transform IR Spectroscopy (FTIR)  Advanced technique.  Interferometer(Michelson Interferometer). 24 11/12/16Chetan Jain
  • 26. InterpretatIon of Ir Spectr 26 11/12/16Chetan Jain
  • 27. applIcatIonS of Ir and ft Ir  Qualitative application  Quantitative application. 27 11/12/16Chetan Jain
  • 28. References  Pharamceutical analysis by A.V. Kasture, S.G. Wadodkar,K.R. Mahadik, H.N. More, Volume II, Nirali Prakashan, Eleventh edition (2004), p.no. 207-221.  Fundamental of analytical chemistry by D.A.Skoog, D.M.West,F.J.Holler,7th edition p.no.592-597.  Organic Spectroscopy by William Kemp, 3rd edition, Palgrave Publication, p.no19-56.  Instrumental Methods of Analysis by H.A.Willard, L.L.Merritt, J.A.Dean, F.A. Settle, 7th edition, p.no. 288 to 320. 28 11/12/16Chetan Jain