INFRARED SPECTROSCOPY

Pn. Suryati Bt. Syafri

En. Maywan Hariono
2009
 What is IR light?
• Is a kind of electromagnetic radiation which
has wave region longer than visible light, but
shorter than radio wave.
• Low energy
 What is IR region?

• The wavelength region is 2.5-25 µm

• The unit commonly used is wavenumbers (cm-
1 ) i.e. 4000-400 cm-1

• Remember that Wavenumber is proportional

with energy (E) and frequency (v), but
reciprocal with wavelength.
Light & Electromagnetic Spectrum
 IR Application
• Broadly applied in several area sort of :
- Army
- Fire man
- Veterinary
- Pharmacy
- Electronic devices
- Remote sensing
 IR spectrum
• Divided into 3 regions
1. Near Infrared
2. Middle Infrared
3. Far Infrared
 Spektrum IR

Ranges Far Middle Near

Infrared Infrared Infrared

Wavelength 50-1000µm 2.5-50µm 0.8-2.5µm

range

Wavelength 200-10cm-1 4000- 12500-

number 200cm-1 4000 cm-1

Energy 0.025- 0.5- 1.55-0.5eV

range 0.0012eV 0.025eV
 Principles
• When the certain molecules are exposed to IR light,
it will absorb the energy to make the atoms of
molecules vibrating
• The vibration frequency depend on the amount of
atoms and the length and the strength of atomic
bonding
• Molecule vibration is stimulated by absorption
radiation in the same frequency with the frequency
of its origin vibrations
 Energy Trends
• Energy follows vibration frequency of atoms
• -light atoms vibrate more rapidly: -CH, NH, OH
vibrations . 2800 cm-1
• Multiple bonds vibrate more rapidly:
triple bonds : C≡C (2100-2200), C≡N (2240-
2280)
Double bonds : C=O (1680-1750), C=C
(1620-1680)
Single bond : C-O (1025-1200)
 Intensity Trends
• Follows change in dipole caused by vibrating atoms
– Polar bonds (strong bond dipoles) absorb strongly
• O-H
• C=O, C=N
• C-O
– Nonpolar bonds absorb weakly
• C=C, C≡C
• Follows overlapping bands
– CH bands tend to overlap
– Molecules contain many CH
– CH absorptions tend to be strong
 PRINCIPLES
• For each molecules, there is a various kind of
vibration occurs
 What kind of sample be able to absorb IR
radiation?
• Only vibration which alters molecule dipole moment (electron
Hanya getaran yang meyebabkan perubahan dipole molekul
(the magnitude of positive and negative charge between two
bonded atoms) and having the IR absorption frequency in the
IR region

• Gas molecules such as O2, H2 and Cl2 don’t have a dipole

moment, means no IR absorption occurs

• SO2 dan CO2 have a dipole moment so it will give IR

absorption
• Every functional group has their own IR absorption
• The more complex in molecule structure, the more
complex in IR absorption
• It is used to identify any functional group presents in
a molecule structure
 IR Spectrum Distribution
1. 4000-2500 cm-1, absorption of atom which is bond
to H atom, ex: C-H, O-H dan N-H
2. 2500-2000 cm-1, triple bond, ex: C≡C , C≡N
3. 2000-1500 cm-1, double bond, ex: C=O, C=C, C=N
4. 1500-400 cm-1, an absorption that involves the
deformation of other bondings
 Fingerprint region (<1500 cm-1)
• Many bands & many overlaps
– Heavy atom stretches
– All bends, etc.
– Should have simple molecule (or other evidence
or structure) before intepreting bands in this
region
• Overall pattern reflects molecular structure
– Pattern from 1400-600 = molecular fingerprints
 Prosedure

• IR light is passed through the sample, and the amount of energy which is absorbed by the
sample per cm wavelength will be recorded .
• The IR light desired will be selected by monochromator before exposed to the sample’
Interferometer is used for measuring all wavelength in one running time.
• The data will be translated into the graph which is plotted as wavelength vs transmision
• The graph might be compared to known standard reference
 Instrumentation
• Conventional method(dispersive instrument)
– The monochromator being used to select
frequency of one radiation in one time through
the sample.
 Peralatan
• Spektrometer FTIR (Fourir Transform IR)
– Semua frekuensi yang diperlukan melalui instrument sekaligus
– Menggunakan interferometer contohnya Michelson Interferometer
– Teknik cepat dan pantas
– Digunakan dikebanyakan makmal kimia
Animation of FTIR
 IR Components
• A. IR Resources
– Quartz halogen
Nernst Glower lamp (run at 2000oC)
– Globar (made from Carbide silicon, run at 1100oC)
 IR Components
• B. sample
• 1. solids
– A. Nujol mull
• The sample is ground using a mortar and pestle to give a very fine
powder
• A small amount is then mixed with nujol (liquid paraffin) togive a
paste
• Several drops of this paste are then applied between two sodium
chloride plates (these do not absorb infrared in the region of
interest)
• The plates are then place in the instrument sample holder ready
for scanning
 IR Components
• B. Potassium Bromide disk
– A verry small amount of the solid (approximately 1-2 mg) is
added to pure potassium bromide powder (approximately
200 mg) and ground up as fine as possible
– This is then placed in a small die and put under pressure
mechanically. The pressure is maintained for several
minutes before removing the die and the KBr disk formed
– The disk is then placed in a sample holder ready scanning
Sample preparation
 Sample preparation
• 2. thin films
– The infrared spectrum of thin film can be easily obtained by placing a
sample in a suitable holder, such as a card with a slot cut for the
sample window
– This method is often used for checking the calibration of an
instrument with a polystrirene sample as the band produced by this
material are accurately known
• 3. liquids
– This is possibly the simplest and the common method for sample
preparation
– A drop of the sample is placed between two potassium bromide or
sodium chloride circular plates to produce a thin capillary film
– The plates are then placed in a holder ready for analysis
 Sample preparation
• 4. gases
– To obtaine an infrared spectrum of a gas requires
the use of a cylindrical gas cell with windows at
each end composed of an infrared inactive
material such as KBr, NaCl or CaF2
– The cell usually has an inlet and outlet port with
atap to enable the cell to be easilly filled with the
gas to be analyzed
 instrumentation
• C. monochromator/interferometer
– Break down the radiation of light to the different
wave region in one time running process.
• D. detector
– CCD (charge couple device)
– InGaAs (Indium Gallium Arsen)
– Pbs (Lead sulfide)
 Instrumentation
• Display
– Exhibit the collected data
– Translate the data to the graph
– The graph is plotted as transmision vs frequnecy
(wavenumbers)
 Advantages
• Provide the fingerprint for the sample being
analyzed
• The installation of instrument to the computer
allows the comparison of sample spectrum
and standard reference can be run
simultaneously
 Disadvantages
• Rarely used for quantitative purpose since the
spectrum produced is too complicated to
determine one by one
• The sample preaparation is quite difficult,
needs the skill to handle it.
aniline
phenol
Salycilic acid
ethanol
 Contoh spektrum
• allopurinol
• phenytoin
 References
• David G. watson (2005). Pharmaceuthical
Analysis. Second edition. Pp:115-128
• http://en. Wikipedia.org./wiki/Infrared
spectroscopy
• http://www.chem.ualberta.ca/~orglabs/proce
dures/Infrared
Spectroscopy/ir/IR%20Main.html