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SPECTROSCOPY
MOHAMED NIJAS V
S5
I.S.P
CONTENT
SPECTROSCOPY.
IR SPECTROSCOPY.
MOLECULAR VIBRATIONS.
EXPERIMENTAL SETUP.
FUTURE DIRECTIONS.
SPECTROSCOPY???
Method of Seeing the unseeable
E
M
R
Atoms
Molecules
ANALYTE
SPECTROPHOTOGRAPH
Conc. should be
lower
1.UV-Visible radiations--------excitation of electrons---------UV-visible spectrum
2.IR-radiations------------------vibration changes in electrons--------IR spectrum
3.Radio frequency---------------spin rotational changes-------------N.M.R spectrum
IR SPECTROPHOTOMETRY
Energy of molecule = Electronic energy+
Vibrational energy + Rotational energy
Concerned with the study of absorption of infrared
radiation, which causes vibrational transition in the
molecule.
Thus known as Vibrational spectroscopy.
Mainly used in structure elucidation to determine
the functional groups.
IR region: 0.8
m (800nm) to
1000 m (1mm)
Near IR: 0.8-2
m
PRINCIPLE OF IR SPECTROSCOPY
Molecules are made up of atoms linked by chemical bonds.
MOLECULAR VIBRATIONS
Stretching vibrations
Vibration or oscillation
along the line of bond
Change in bond length
Occurs at higher energy:
4000-1250 cm-1
a) Symmetrical stretching
b) Asymmetrical stretching
Bending vibrations
Vibration not along the
line of bond
Bond angle is altered
Occurs at low energy:
1400-666 cm-1
a) In plane bending
b) Out plane bending
STRECHING VIBRATIONS
a) Symmetrical stretching:
2 bonds increase or decrease in length simultaneously.
H
b) Asymmetrical stretching
in this, one bond length is increased and other is decreased.
a) In plane bending
i. Scissoring:
. 2 atoms approach each other
. Bond angles are decrease
H
C
H
ii. Rocking:
. Movement of atoms take place in the same direction.
EXPERIMENTAL SETUP
COMPONENTS
1. Source
2. Fore optics
3. Monochromator
4. Detector
5. Recorder
SOURCE
Ideal => black body radiator
COMMONLY USED =>globar FILAMENT &NERNST GLOWER
Globar- resistance rod of silicon carbide
Nernst glower-a spindle of rare earth
oxide(thorium,zirconium,etc)
Globar-for longer wavelengths
Nernst glower-for shorter wavelengths
FORE OPTICS
CONSISTS OF SOURCE,MIRRORS
M1,M2 AND A ROTATING MIRROR M
M1,M2 DIVIDES THE BEAM
M ALTERNATELY ALLOWS
THESAMPLE BEAM AND
REFERENCE BEAM TO PASS
THROUGH
MONOCHROMATOR
Splits the polychromatic readiation to component
wavelengths.
Make use of prisms or grating or both.
Resolution depends on slit width and quality of mirrors.
Rock salt prism is generally use d in the range of 6504000cm-1
DETECTOR
Measure the radiant energy by its heating effect.
Thermopiles bolometer and golay cells are generally used
Photoconductivity is also used.
Radiation is allowed to fall on photo conducting material and the
conductivity of the material is measured continuously by a bridge network.
Once the sample absorbs radiation, there will be inequality between the
two radiations and signal will be produced.
THE RECORDER
The amplified signal is used to move an attenuator which cuts
down the radiation coming out of the reference beam until
energy balance is restored.
This is achieved by a motor which drives the comb into the
reference beam when an absorbing band is encountered and
out of the beam when the band is passed over.
The recorder pen is also coupled to this motor so that the
comb movement is followed exactly y the pen