Presented by:
Himani peshavaria
19-PCH-055
Msc analytical chemistry sem 3.
Dispersive IR Spectrophotometer
Contents
 Principle
 Instrumentation
 Working
 Applications
 Disadvantages
Principle
 IR Spectroscopy detects frequencies of infrared
light that are absorbed by a molecule.
 Molecules tend to absorb these specific
frequencies of light since they correspond to the
frequency of the vibration of bonds in the
molecule.
 The energy required to excite the bonds
belonging to a molecule, and to make them
vibrate with more amplitude, occurs in the
Infrared region.
 A bond will only interact with the electromagnetic
infrared radiation, if it is polar.
Instrumentation
 An IR spectrometer consists of three basic
components:
1. Radiation source.
2. Monochromator.
3. Detector.
1) Radiation source
 The common radiation source for the IR
spectrometer is an inert solid heated electrically
to 1000 to 1800 °C.
 Three popular types of sources are :
a) Nernst glower (constructed of rare-earth
oxides),
b) Globar(constructed of silicon carbide),
c) and Nichrome coil.
a) Nernst glower
 It is composed of rare earth oxides e.g.,
zirconium oxide , yttrium oxide.
 It consists of a hollow rod with a diameter of 1 to
2 mm and a length of perhaps 20 mm.
 Platinum ends leads to passage of electricity.
 It is non conducting at room temperature and
must be heated by external means to bring it to a
conducting state.
 Advantage is that it produces intense IR radiation
and IR range is also wide.
 Disadvantage of Nernst glower is its frequent
mechanical failure.
b) Globar
 It is a rod of silicon carbide, usually about 5 cm in
length and 0.5 cm in diameter.
 It is heated to a temperature between 1300 and
1700 °C.
c) Nichrome coil.
 It produces a lower intensity of radiation than the
Nernst or Globar sources, but has a longer
working life.
 The wire source is a tightly wound coil of
nichrome wire.
 Electrically heated to 1100 °C.
2) Monochromators
 Monochromator splits polychromatic light into
monochromatic light.
 They are mainly of two types:
a) Prism monochromators.
b) Grating monochromators.
a) Prism
 Several materials are used for the construction of
prism.
 Quartz is employed for near IR region.
 Crystalline sodium chloride is the most common
prism material.
 Its dispersion is high between 5-15 μm.
 Crystalline potassium bromide and
cesium bromide provide prism
materials for far IR.
 Lithium fluoride is useful
for near ir region.
b) Grating
 A grating is a device that consists of a series of
identically shaped, angled grooves.
 Gratings for the infrared region have a much
wider spacing between the grooves.
3) Detectors
 Most detectors used in dispersive IR
spectrometers can be categorized into two
classes:
a) photo detectors : they use the quantum effect of
the infrared radiation to change the electrical
properties of a semiconductor.
b) Thermal detectors : IR radiation produces a
heating effect that alters some physical property
of the detector.
a) Photo detectors
 They are constructed from semi conductor
crystals such as lead sulfide, lead selenide and
germanium.
 Absorption of radiation by these materials results
in excitation of non conducting electrons to an
excited conducting state.
 The increase in conduction or decrease in
resistance can be readily measured and is
directly related to the number of photons reaching
the semiconductor surface.
b) Thermal detectors
 Thermal detectors are mainly of three types :
1. Thermocouple
2. Bolometer
3. Golay cell
1) Thermocouple
 Thermocouple consists of a pair of junction of different
metal wires.
 The potential difference (voltage) between the junctions
changes according to the difference in temperature
between the junction.
 Hence, current flow which is altered is recorded by the
recorder.
2) Bolometer
 It consist of a thin metal conductor
 When radiation falls on this conductor, its temperature
changes, as the resistance of a metallic conductor
changes with temperature.
 When no radiation falls on the bolometers, the bridge
remains balanced.
 If radiation falls on the bolometers, the bridge become
unbalanced due to changes in the electrical resistance
which causes a current to flow through the
3) Golay cell
 It consists of a small metal
cylinder which is closed by a
blackened metal plate at one end
and by a flexible metalized
diaphragm at the other.
 After filling the cylinder with
xenon, it is sealed.
 When IR radiation is allowed to
fall on the blackened metal plate,
it heats the gas which causes it
to expand.
 The signal seen by the device is
modulated in accordance with
the power of the radiant beam
Working
 Two equivalent beams from the same source
pass through the sample and reference chambers
respectively.
 Using an optical chopper, the reference and
sample beams are alternately focused on the
detector.
 Commonly, the change of IR radiation intensity
due to absorption by the sample is detected as a
signal that is translated into the recorder
response through the actions of synchronous
motors.
Applications
 Identification of all types of organic and many
types of inorganic compounds.
 Determination of functional groups in organic
materials.
 Determination of molecular orientation .
 Determination of molecular conformation
(structural isomers) and stereochemistry (
geometrical isomers ).
Disadvantages
 Slow scan speed make dispersive instruments
too slow for monitoring systems undergoing rapid
changes .
 Less sensitivity .
 Many moving parts may results in mechanical
slippage .
 Accuracy is less compared to Fourier Transform
IR(FTIR) .
References
 Introduction to Spectroscopy Book by Donald L.
Pavia, Gary M. Lampman, and George S. Kriz
 Handbook of Instrumental Techniques for Analytical
Chemistry Book by Frank A. Settle.
 Principles of Instrumental Analysis 6th Edition
by Douglas A. Skoog , F. James Holler , Stanley R.
Crouch .
 http://www.authorstream.com/Presentation/vvkvjoshi
-1948442-dispersive-ir-spectrophotometer/
 http://delloyd.50megs.com/MOBILE/infrared_spectro
scopy.html
 spectroscopyinstrumentationby-dr-
190618085453.pdf
Dispersive ir spectrophotometer

Dispersive ir spectrophotometer

  • 1.
    Presented by: Himani peshavaria 19-PCH-055 Mscanalytical chemistry sem 3. Dispersive IR Spectrophotometer
  • 2.
    Contents  Principle  Instrumentation Working  Applications  Disadvantages
  • 3.
    Principle  IR Spectroscopydetects frequencies of infrared light that are absorbed by a molecule.  Molecules tend to absorb these specific frequencies of light since they correspond to the frequency of the vibration of bonds in the molecule.  The energy required to excite the bonds belonging to a molecule, and to make them vibrate with more amplitude, occurs in the Infrared region.  A bond will only interact with the electromagnetic infrared radiation, if it is polar.
  • 4.
    Instrumentation  An IRspectrometer consists of three basic components: 1. Radiation source. 2. Monochromator. 3. Detector.
  • 5.
    1) Radiation source The common radiation source for the IR spectrometer is an inert solid heated electrically to 1000 to 1800 °C.  Three popular types of sources are : a) Nernst glower (constructed of rare-earth oxides), b) Globar(constructed of silicon carbide), c) and Nichrome coil.
  • 6.
    a) Nernst glower It is composed of rare earth oxides e.g., zirconium oxide , yttrium oxide.  It consists of a hollow rod with a diameter of 1 to 2 mm and a length of perhaps 20 mm.  Platinum ends leads to passage of electricity.
  • 7.
     It isnon conducting at room temperature and must be heated by external means to bring it to a conducting state.  Advantage is that it produces intense IR radiation and IR range is also wide.  Disadvantage of Nernst glower is its frequent mechanical failure.
  • 8.
    b) Globar  Itis a rod of silicon carbide, usually about 5 cm in length and 0.5 cm in diameter.  It is heated to a temperature between 1300 and 1700 °C.
  • 9.
    c) Nichrome coil. It produces a lower intensity of radiation than the Nernst or Globar sources, but has a longer working life.  The wire source is a tightly wound coil of nichrome wire.  Electrically heated to 1100 °C.
  • 10.
    2) Monochromators  Monochromatorsplits polychromatic light into monochromatic light.  They are mainly of two types: a) Prism monochromators. b) Grating monochromators.
  • 11.
    a) Prism  Severalmaterials are used for the construction of prism.  Quartz is employed for near IR region.  Crystalline sodium chloride is the most common prism material.  Its dispersion is high between 5-15 μm.  Crystalline potassium bromide and cesium bromide provide prism materials for far IR.  Lithium fluoride is useful for near ir region.
  • 12.
    b) Grating  Agrating is a device that consists of a series of identically shaped, angled grooves.  Gratings for the infrared region have a much wider spacing between the grooves.
  • 13.
    3) Detectors  Mostdetectors used in dispersive IR spectrometers can be categorized into two classes: a) photo detectors : they use the quantum effect of the infrared radiation to change the electrical properties of a semiconductor. b) Thermal detectors : IR radiation produces a heating effect that alters some physical property of the detector.
  • 14.
    a) Photo detectors They are constructed from semi conductor crystals such as lead sulfide, lead selenide and germanium.  Absorption of radiation by these materials results in excitation of non conducting electrons to an excited conducting state.  The increase in conduction or decrease in resistance can be readily measured and is directly related to the number of photons reaching the semiconductor surface.
  • 15.
    b) Thermal detectors Thermal detectors are mainly of three types : 1. Thermocouple 2. Bolometer 3. Golay cell
  • 16.
    1) Thermocouple  Thermocoupleconsists of a pair of junction of different metal wires.  The potential difference (voltage) between the junctions changes according to the difference in temperature between the junction.  Hence, current flow which is altered is recorded by the recorder.
  • 17.
    2) Bolometer  Itconsist of a thin metal conductor  When radiation falls on this conductor, its temperature changes, as the resistance of a metallic conductor changes with temperature.  When no radiation falls on the bolometers, the bridge remains balanced.  If radiation falls on the bolometers, the bridge become unbalanced due to changes in the electrical resistance which causes a current to flow through the
  • 18.
    3) Golay cell It consists of a small metal cylinder which is closed by a blackened metal plate at one end and by a flexible metalized diaphragm at the other.  After filling the cylinder with xenon, it is sealed.  When IR radiation is allowed to fall on the blackened metal plate, it heats the gas which causes it to expand.  The signal seen by the device is modulated in accordance with the power of the radiant beam
  • 19.
    Working  Two equivalentbeams from the same source pass through the sample and reference chambers respectively.  Using an optical chopper, the reference and sample beams are alternately focused on the detector.  Commonly, the change of IR radiation intensity due to absorption by the sample is detected as a signal that is translated into the recorder response through the actions of synchronous motors.
  • 21.
    Applications  Identification ofall types of organic and many types of inorganic compounds.  Determination of functional groups in organic materials.  Determination of molecular orientation .  Determination of molecular conformation (structural isomers) and stereochemistry ( geometrical isomers ).
  • 22.
    Disadvantages  Slow scanspeed make dispersive instruments too slow for monitoring systems undergoing rapid changes .  Less sensitivity .  Many moving parts may results in mechanical slippage .  Accuracy is less compared to Fourier Transform IR(FTIR) .
  • 23.
    References  Introduction toSpectroscopy Book by Donald L. Pavia, Gary M. Lampman, and George S. Kriz  Handbook of Instrumental Techniques for Analytical Chemistry Book by Frank A. Settle.  Principles of Instrumental Analysis 6th Edition by Douglas A. Skoog , F. James Holler , Stanley R. Crouch .  http://www.authorstream.com/Presentation/vvkvjoshi -1948442-dispersive-ir-spectrophotometer/  http://delloyd.50megs.com/MOBILE/infrared_spectro scopy.html  spectroscopyinstrumentationby-dr- 190618085453.pdf