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PRESENTATIO
N
INTRODUCTION
Infrared spectroscopy (IR
spectroscopy) is the subset of
spectroscopy that deals with the
infrared region of the
electromagnetic spectrum. It covers
a range of techniques, the most
common being a form of
absorption spectroscopy. As with
all spectroscopic techniques, it can
be used to identify compounds or
PRINCIPLE
Bond strength
Mass of atoms
Hydrogen bonding
Electronegative atoms
Conjugation
Interpretation of spectrum
Between 3650-3100per cm,the
functional groups OH and NH
appear
Around 1700per cm,the C=O absorbs
I.R radiation
Around 1600per cm,the C=C
stretching of unsymmetrical alkenes
and aromatics and carbon nitrogen
stretching occurs at this
wavenumber
Interpretation of
spectrum(contd)
The fingerprint region is
characteristic of the molecule as a
whole and is observed between
1500-650per cm.
PROCEDURE
Sample preparation
Gaseous samples require little
preparation beyond purification, but
a sample cell with a long pathlength
(typically 5-10cm) is normally
needed, as gases show relatively
weak absorbances.
INSTRUMEINTATION
we will be limiting our attention to
instrumentation concerned with
spectroscopy in the middle region
(4000 - 200cm-1). It is absorption in
this region which gives structural
information about a compound
The chopper arranges for the sensor to alternately receive light that has
been transmitted through the cell, and light that has passed through
the attenuator. The servo system of the attenuator adjusts the light
transmission until both beams have the same intensity. The amount of
light that is absorbed is indicated by the position of the attenuator.
More simply, the amount of light of the chosen wavelength which is
absorbed by the sample, is measured by attenuating the reference
beam until its intensity is equivalent to that of the beam transmitted
through the sample. The resolution is controlled by the width of the slit
which is adjustable. In the older versions of this type of IR spectrometer,
an analog plotter, mechanically associated with the attenuator,
recorded the spectrum. Even if modified to provide an output that is
proportional to absorption, the big disadvantage of this type of
spectrometer for use in combined systems is its very slow rate of
scanning.
SOURCES
DETECTORS
Thermocouples consist of a pair of junctions of
MONOCHROMATORS
May be either a prism or grating.
Most common prisms material is
NaCl (transparent from 4000-650cm1). Suffers from low resolution
KBr may be used (extends range to
400)
Other CsBr, CsI
types
Dispersive infra red spectophotometers
These are often double-beam recording
instruments, employing diffraction gratings for
dispersion of radiation.
Radiation from the source is flicked between the
reference and sample paths. Often, an optical null
system is used. This is when the detector only
responds if the intensity of the two beams is
unequal. If the intensities are unequal, a light
attenuator restores equality by moving in or out of
the reference beam. The recording pen is attached
to this attenuator
Adv.
Improved frequency resolution
Improved frequency reproducibility (older
dispersive instruments must be recalibrated for
each session of use)
Higher energy throughput
Faster operation
Computer based (allowing storage of spectra and
facilities for processing spectra)
Easily adapted for remote use (such as diverting
the beam to pass through an external cell and
detector, as in GC - FT-IR)
MODERN
ADVANCEMENT
OUTGAS 6 FTIR
APPLICATION
IDENTITY
Substances that give the same IR Spectra are
CONFIRMATON OF IDENTITY
Most IR Spectra especially in the fingerprint
region(1500-650) contain some considerable
detail and direct comparison of two spectra
which have been recorded under the same
sampling conditions offers one of the most
reliable ways of examining the identity or
unidentity of two samples
Detection of IMPURITIES
IR may prove to be useful if only the
impurity absorbs strongly in a
regionwhere the main component is
reasonably transparent eg.
Adrenalone in adrenaline
Recognition of functional
groups
The IR Spectrum is capable of yielding
Recog cont
This makes IRSpectrum the
QUANTITATIVE ANALYSIS
The application of IR for quantitative
analysis has diminished with the
advent of newer techniques such as
Gas Chromatography,HPLC,NMR and
Spectrofluorimetry.
Quantitative cont
The quantitative analysis is based on
the fact that the intensity or depth of
an absorption band in a substances
is reflected to the concentration of
the material associated with that
band
QUANTITATIVE ANALYSIS
CONTD
For solutions (of drug formulations)
the Beer Lamberts law holds and
since the IR Spectrophotometers
measures band intensities linearly in
%T and therefor log.in Absorbance,A.
cont
A plot of Absorbance against concentration
for a series of standards using a calibration
curve, the absorbance of the unknown can
be measured and the curve used to read
the concentration and vice versa.eg
determination of amount of
phenobarbitone in phenobarbitone tablets.
QUANTITATIVE CONTROL OF
CHEMICAL RXN AND SEPARATION
IR provides a convenient and simple method
for checking each stage of synthesis or for
monitoring Chromatographic Separation or
progress of organic reactions especially if
they involve suitable spectral changes
eg.include the oxidation of a secondary
alcohol(3570cm-1) to ketone (1725cm-1)and
chromatographic separation of a 5membered-ring ketone(1750cm-1)and a 6memberedisomer(1750cm-1)