Vibrational Spectroscopies and NMR

Vibrational Spectroscopy
and NMR
:By
Suha Qais Muhammed Hasan

Vibrational Spectroscopies and NMR
 Fourier transform infrared spectroscopy (FTIR)

 Raman spectroscopy
 High resolution electron energy loss
spectroscopy (HREELS)
 Solid state nuclear magnetic resonance (NMR)
Fourier transform infrared spectroscopy
What is FTIR Spectroscopy?
 FTIR spectroscopy (FTIR) is an analytical methodology used in
industry and academic laboratories to understand the structure
of individual molecules and the composition of molecular
mixtures.
 FTIR is the study of interactions between matter and
electromagnetic fields in the IR region. A common FTIR
spectrometer consists of a source, interferometer, sample
compartment, detector, amplifier, A/D convertor, and a
computer.
Fourier transform infrared spectroscopy
What is the principle of FTIR Spectroscopy ?
 Broad band infrared energy from the source is directed onto a
beamsplitter, which passes the energy along two different paths.
One path has a fixed mirror at the end and the other has a moving
mirror.
 The infrared energy from these two paths return and recombine at
the beamsplitter causing a constructive and destructive interference
pattern, the interferogram. This modulated infrared beam is passed
to the sample where it is absorbed as a function of the molecular
structure of the sample.
 The resultant interferogram is treated with a Fourier transform that
convert it. The single beam sample spectrum resulting in the
typical infrared absorbance/transmission spectrum.
Fourier transformation infrared
spectroscopy
Illustration graph for (FTIR) spectroscopy
Transmission FTIR and Reflection FTIR
Transmission FTIR
 The incident radiation does not pass through an IRE crystal to interact with a
sample species. IR light passes directly into a solid, liquid or gaseous sample where
a specific wavelength or frequency of light will be absorbed by the sample.
 Economical but Sample preparation can be difficult.

 Well established, most traditional form of sample measurement.
 Excellent spectral information.
 Great for quantitative work – many standard operating procedures are based on
transmission.
 Excellent for solids, liquids and gases.
Transmission FTIR and Reflection FTIR
Reflection FTIR
 Collect light reflected from an interface air/sample,
solid/sample or liquid/sample
 Analyze liquids, solids, gels or coatings
 Minimal sample preparation
 Convenient for qualitative analysis.
Applications of FTIR
 It can determine the amount of component in mixture.
 The effect of curing a material can be observed by peak-width
analysis. As one anneals defects, the bands become narrower
and more intense.
 It is use in the analysis of molecules important in the
pharmaceutical, chemical and polymer industries. It is used in
industry and academic laboratories.
 It is used in environmental and water quality analysis.
Advantages and limitations of FTIR
Advantages:
1. FTIR, spectrum can be obtained very quickly and saves time(It generally
completes a scans within 1 to 2 seconds), with high resolution.
2. Gases, solids as well as liquid can be analyses with FTIR.
3. FTIR is non-destructive technique.
4. Organic compounds and Inorganic compounds can be identified easily
using FTIR.
5. FTIR can identify even small concentrations of contaminants.
Limitations:
It is not possible to know the molecular weight of substance.
Video about FTIR
Raman spectroscopy
 Is a spectroscopic technique typically used to determine
vibrational modes of molecules.
 Raman spectroscopy is commonly used in chemistry to provide
a structural fingerprint by which molecules can be identified.
 The Raman process that excites molecular and crystal vibrations
is called Stokes scattering, the process that annihilates existing
vibrations is called anti- Stokes scattering.
 The molecule should be in a higher energy state to generate
anti-Stokes Raman photon and it may be caused by thermal
excitation.
 The anti-Stokes Raman scattering is substantially weaker than
the Stokes Raman scattering but has the advantage that it is less
affected by the luminescence background.
Raman spectroscopy
Principle of Raman Spectroscopy
The process involves the inelastic scattering of a beam of monochromatic light
by a sample material. Usually, a laser is used for generating this light that interacts
with vibrating molecules, phonons or other stimulations in the system. This results
in shifting the energy level of the laser photons to oscillate up and down and give
information about the vibration patterns of the system, a phenomenon called the
Raman Effect.
Sample requirements in Raman
spectroscopy
 Liquids: Liquids and solutions can be
measured in special cells that have optical
windows at right angles, or they can be
contained in capillary tubes or small vials.
 Powder and polycrystalline solids:
Usually, particle size has relatively little
effect on Raman line shapes unless the
particles are extremely small, less than
100 nm.
 Single-Crystal Measurement: Maximum
information is obtained by making Raman
measurements on oriented, transparent
single crystals.
Applications of Raman spectroscopy
 it is use for Microscopic Analysis.

 Detecting Crystal Structure.
 learn about the properties for gaining an
advantage in nanoelectronics and in making
nano-sensors.
 examine powders and tissues.
Advantages and limitations of Raman
spectroscopy
Advantages:
• No sample preparation required.
• Smaller sampling (1 micron or less is possible).
• Non destructive.
• Standard detector can be used.
• Very suitable for biological sample.
Limitations:
• Scattering signal is weak.
• Environment, temperature, vibration, …etc., may affect on the
laser.
Video about Raman spectroscopy
High Resolution Electron Energy Loss
Spectroscopy (HREELS)
 High resolution electron energy loss spectroscopy (HREELS)
is a tool used in surface science. The inelastic scattering of
electrons from surfaces is utilized to study electronic
excitations or vibrational modes of the surface of a material
or of molecules adsorbed to a surface.
 The main reasons for the popularity of HREELS over optical
methods are its very small detection limit and its wide
spectral range at high surface sensitivity.
The principle of HREELS
In High-Resolution Electron Energy Loss Spectroscopy
(HREELS), a highly mono energetic beam of low energy is
focused onto a sample’s surface, and the scattered
electrons are analyzed with high resolution of the scattering
energy and angle.
A vibrational spectrum can be obtained by counting the
number of electrons versus the electron energy loss relative
to the elastically scattered (no energy loss) electron beam.
This spectrum is used mainly to identify chemical species
(functional groups) in the first layer of the surface.
Scheme about HREELS
Applications of HREELS
1. Used to obtain information on the chemical composition,
morphology, structure, and phonon modes of the solid
surface.
2. Functional groups on polymer and polymer film surface.
3. Concentrations of free charge carriers in semiconductors.
4. Adsorbed species on single crystal surfaces.
Solid State Nuclear Magnetic
Resonance (NMR)
 Solid state NMR is a relatively recent spectroscopic technique
that can be used to uniquely identify and quantitate
crystalline phases in bulk materials, at surfaces and interfaces.
NMR resembles X-ray diffraction in this capacity.
 NMR spectroscopy exploits the magnetism of certain nuclear
isotopes.
 Nuclei with odd mass, odd atomic number, or both possess a
permanent magnetic moment, which can be detected by
applying an external magnetic field.
The principle of solid state NMR
 A sample placed in a magnetic field develops a macroscopic
magnetization. This magnetization forms the source of the
spectroscopic signal measured.
 In NMR spectroscopy the precise energy differences between
such nuclear magnetic states are of interest. To measure these
differences, electromagnetic waves in the radiofrequency region
(1-600 MHz) are applied, and the frequency at which transitions
occur between the states, is measured.
 NMR experiments can be carried out on solid samples in any
form.
 Sample preparation requirements in solid state NMR are
strikingly simple because the measurement is carried out at
ambient temperature and pressure.
Solid State Nuclear Magnetic
Resonance (NMR)
Applications of Solid State
(NMR)
 A most recent development has been the successful
demonstration of three-dimensional imaging of ceramic
and polymeric materials by solid state NMR techniques.
 Also it is used in characterization of thin film, glasses,
composite and many metals.
Advantages and limitations of solid
state NMR
Advantages:
 Sample preparation requirements in solid state NMR are strikingly simple
because the measurement is carried out at ambient temperature and
pressure.
 NMR experiments can be carried out on solid samples in any form, as far
as the sample dimensions fit those of the coil in the NMR probe.
 Compared to other spectroscopic methods, NMR spectroscopy is a very
insensitive technique.
Limitations:
low sensitivity poses a particular obstacle to NMR studies of thin films and
surfaces.
Due to the use of magnetic field in this method, so many element in the
periodic table can be considered generally unsuitable for solid state NMR.
Video about solid state NMR
Comparison between Vibrational Spectroscopy
methods and NMR
Any questions?
Thanks for your
attention

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Vibrational Spectroscopy

 Fourier transform infrared spectroscopy (FTIR)

 Economical but Sample preparation can be difficult.

 it is use for Microscopic Analysis.

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