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Ir Spectroscopy 3
Ir Spectroscopy 3
Ir Spectroscopy 3
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Gas cells
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2- Liquids & Solutions:
A neat sample may be examined as a thin film
(0.1mm thickness) squeezed between two
optically polished circular flat plates (5mm
thickness & 25mm diameter) of rock salt
(NaCl, KBr).
The plates held together by capillary action &
mounted in the sample beam.
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Plates must be cleaned immediately after use
by rinsing with suitable solvent (chloroform),
kept dry, store in well closed desiccator &
should be handled by their edges.
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3- Solids:
Two common techniques for solid sample,
mulls & pellets.
a) Mulls:
The finely ground solid sample (2-10mg)
mixed with Nujol (mineral oil) to make a thick
paste, which is spread b/w 2 plates (alkali halides).
Then mounted in a path of infrared beam & the
spectrum is run.
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b) Pellet:
Finely ground sample is thoroughly mixed
with same wt of powdered KBr.
The mixture is then pass under high pressure
(8000-20,000 psi) in a press (13mm diameter) to
form a small pellet (transparent).
An evacuable, heated (40°c) metal desiccator
is useful for storing die components & KBr.
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FTIR sampling compartment
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Qualitative Analyses, Structural Determination &
Interpretation
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Conti..
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Interpretation of IR Spectra
The 1st region to look at is the 4000–1300 cm-1
region, called the functional group region.
This is the region where strong absorptions
due to stretching from the hydroxyl, amine,
carbonyl & CHx groups occur.
This region also has areas of weak absorptions
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that are very informative. The 2000–1660 cm
region will show a set of weak overtone if an
aromatic ring is present.
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Conti..
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Aromatic Hydrocarbons:
Benzene C6H6 an aromatic hydrocarbon.
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5- Percentage composition of a mixture:
If Beer’s law is obeyed, the spectrum of
mixture resulting from the known composition
of pure components is determined (multiple
standard).
Then measure the spectra of unknown sample
& by graphic method (% age purity find).
6- Study of atmospheric contaminants:
Infrared spectroscopy has been employed for
variety of compounds for which limits of
exposure have been set by health
administration.
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7- Determination of total amine contents:
The total primary & secondary amine content
of aliphatic amines can be determined easily &
rapidly by functional group analysis in the
near-infrared.
8- Analysis of petroleum, hydrocarbons, oil
& grease contents by EPA:
Semi quantitative determination of petroleum,
hydrocarbons, oils & grease can be done by
comparison of IR spectra of sample with
standards.
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The most common use of IR spectroscopies
are for qualitative identification & structure
determination of organic compounds.
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Quantitative analysis:
IR spectroscopy was considered to provide
only qualitative & semi quantitative analysis of
common samples, particularly when data were
acquired by use of conventional dispersive
instrument.
However, the development of FT-IR
instrumentation & computerized data-
processing capabilities have highly improved
the performance of quantitative IR work.
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The basis for quantitative analysis of
absorption spectrometry is the Beer’s law.
A = αbc
α = molar absorptivity
b = path length
c = concentration
Instead of transmittance scale, absorbance is
used in quantitative analysis, absorbance “A”
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