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Infrared Spectroscopy: Presented by Uttam Prasad Panigrahy M.Pharm
Infrared Spectroscopy: Presented by Uttam Prasad Panigrahy M.Pharm
SPECTROSCOPY
PRESENTED BY
UTTAM PRASAD PANIGRAHY
M.PHARM
CONTENTS
1. INTRODUCTION
2.PRINCIPLE
3. THEORY-MOLECULAR
VIBRATION
4. INSTRUMENTATION
5.IMPORTANT FEATURES
6.APPLICATIONS
Definition:
1m = 10-6 m ;
cm-1 = no. of waves per cm of path
= 1/[ (cm)]
energy of wave
E = h = hc
Infrared region
Molecular vibrations
The positions of atoms in a molecules are not fixed; they are subject to a
number of different vibrations. Vibrations fall into the two main catagories of
stretching and bending.
Stretching: Change in inter-atomic distance along bond axis
Bending: Change in angle between two bonds. There are four types of
bend:
•Rocking
•Scissoring
•Wagging
•Twisting
Vibrational coupling
In addition to the vibrations mentioned above, interaction between
vibrations can occur (coupling) if the vibrating bonds are joined to a
single, central atom. Vibrational coupling is influenced by a number of
factors;
Determines Frequencies
of Infrared Absorbed and
Infrared
plots them on a chart
Source
Infrared
Sample Spectrum
intensity of
Absorption absorption
“peaks”
frequency
(decreasing)
Sources
• Tungsten incandescent lamp – black body source for
measurements in NIR
• Nichrome (or rhodium) wire – Coiled, heated by resistance to
incandescence.
Black oxide layer forms on surface. Temperature 1100°C. Requires little
maintenance and no cooling required. Emits in Mid-IR but less power
than other
sources. Cheaper instruments
• Nernst Glower (rare earth oxides) – More intense emitted
radiation.
Constructed from mixture of fused oxides of Zr, Th and Cs. Non-
conducting at ambient temperatures but at temperatures >800 °C it is
electrically conducting, maintains high temperature by resistive heating.
Good energy output (intensity 2x nichrome wire or globar)
• Globar – A rod of silicon carbide 6-8 mm in diameter.
Characteristics between
nichrome wire and Nernst Glower. Self starting and operates at 1300
°C. Globar
must be water cooled – brass jacket surrounds globar.
• Carbon Dioxide Laser – Useful for narrow radiation bands
Instrumentation-Components
♦ Sample Cells and Preparation
• Solids
• Mull - suspend ground solid in oil of similar refractive index
(Nujol, perfluorocarbon)
• KBr Pellet - few mg sample + 0.5 to 1 g dry KBr ground +
compressed at very high pressure
• Disposable polyethylene film strips (dissolve solid in volatile
solvent,
“paint” on the film or on a salt plate)
• Liquids
• Gases
♦Optics - dessicated salts such as NaCl, CsBr, LiF, KBr and front
surface mirrors. Glass and quartz lenses cannot be used because
they absorb IR radiation
♦Chopper (modulation and tuned amplifier)
Most flexible system for analyzing all 3 states
of matter (solid, liquid, gas)
“Neat” (analysis of liquids/oils)
Pellet (analysis of solids)
Thin Cell (analysis of dissolved solid samples -
solutions)
Long Cell (analysis of gases)
Preparing a “Neat” IR Sample
Preparing a KBr Disk
Apparatus for KBr Disk
Sample cells
Pt leads
cement
1 - 3 mm dia.
SiC rod
heated
to
5 cm 1300oC
water-
cooled
+ temp brass
coeff. of tube
resistance 6 - 8 mm dia. with slot
G 15 m NG 10 m NG 1 m
650 cm -1 G 1000 cm -1 10000 cm -1
Photon detectors
e - p ro m o te d fro m v a le n c e b a n d
to u n fille d c o n d u c tio n b a n d ,
c a u s in g e - h o le p a ir fo rm a tio n .
N o . o f p a irs d e p e n d s o n lig h t
in te n s ity.
p h o to v o lta ic :
p d c a u s e d b y s e p a ra tio n o f e -
h o le p a irs b e tw e e n n , p la y e r.
p h o to c o n d u c tiv e :
R c h a n g e s w ith ra d ia tio n p o w e r,
fo r s e m ic o n d u c to r.
p h o to e le c tro m a g n e tic :
u tilis e H a ll E ffe c t in
s e m ic o n d u c to r.
http://www.chem.vt.edu/chem-ed/scidex.html
Look for C=O peak (1820-1660 cm-1)
If C=O check for OH (3400-2400 cm-1)
◦ indicates carboxylic acid
If C=O check for NH (3500 cm-1)
◦ indicates amide
If C=O check for C-O (1300-1000 cm-1)
◦ indicates ester
If no OH, NH or C-O then ketone
Analyzing IR Spectra
Analyzing IR Spectra
B - CH stretch (2800)
Sample IR Spectrum #1
Sample IR Spectrum #2
C
B
O
C CH3
A
Acetophenone