FTIR
Fourier Transform Infrared Spectroscopy
Purpose:
Specific info. about chemical bonding and molecular structures, making it
useful for analyzing organic materials and certain inorganic materials
•Identifying the molecular structure of organic compounds for
contamination analysis
• Identification of organic particles, powders, films, and liquids
(material identification)
•Can be used to identify functional groups and compounds.
FTIR
Principles:
It involves the absorption of electromagnetic
radiation in the infrared region of the spectrum
which results in changes in the vibrational energy
of molecule.
Since, usually all molecules will be having
vibrations in the form of stretching, bending, etc.,
the absorbed energy will be utilised in changing
the energy levels associated with them.
It is a valuable and formidable tool in identifying
organic compounds which have polar chemical
bonds(such as OH, NH, CH, etc.) with good
charge separation (strong dipoles).
Instrumentation:
It was originally designed as a double beam spectrophotometer
comprising
IR source (red hot ceramic material), grating monochromator,
thermocouple detector, cells made of either sodium chloride or
potassium bromide materials, etc. In this process the light is
dispersed by the monochromator. But, this type of basic design for
IR measurements has been outdated. Instead a newer technique
termed Fourier Transform-Infrared (FT-IR) has been in
practice.
• This technique utilises a single beam of un-dispersed light. In FT-IR, the
un-dispersed light beam is passed through the sample and the
absorbances at all wavelengths are received at the detector
simultaneously.
• A computerized mathematical manipulation (known as “Fourier
Transform”) is performed on this data, to obtain absorption data for each
and every wavelength. To perform this type of calculations interference
of light pattern is required for which the FT-IR instrumentation contains
two mirrors, one fixed and one moveable with a beam splitter in between
them. Before scanning the sample a reference or a blank scanning is
required. The following is the simplified design of the instrument:
Applications:
It finds extensive use in the identification and structural
analysis of organic compounds, natural products,
polymers, etc.
The presence of particular functional group in a given
organic compound can be identified. Since every
functional group has unique vibrational energy, the IR
spectra can be seen as their fingerprints.
Disadvantages:
• Samples containing mixture of substances can
not be analysed.
• Since the sample holders and beam splitter, are
made of moisture sensitive materials like
sodium chloride or potassium bromide (KBr),
special cells are required for aqueous samples
(e.g. KRS-5, ZnSe, etc.).
Water is a bad solvent for IR spectral works.
Characteristic examples
S Product Instruments Results
No Used
1 Rasa XRD Kajjali – peakes due to free sulphur, Mercury oxide& Mercury
sindoor Sulphide
TEM image spongy like structure with the particle size lying in the micro
range
ESCA/XPS Presence of C and O peaks indicating organic coating. Not
detected Mg, Ca, and Fe was shown in EDAX analysis,
indicating their absence on the surface
FTIR spectrum Shows peaks due to organic molecules
2 Naga EDAX Bhasma is found to be rich in Mg, Ca and Fe along with major
Bhasma element Pb
1. Sunil Kumar Singh, Anand Chaudhary, DK Rai & SB Rai, Preparation and characterization of a mercury based
Indian traditional drug Ras-Sindoor, Indian Journal of Traditional Knowledge
Vol. 8 (3), July 2009, pp. 346-351
2. S. K. Singh, D. N. S. Gautam, M. Kumar, and S. B. Rai Synthesis, Characterization and Histopathological Study
of a Lead-
Based Indian Traditional Drug: Naga Bhasma, Indian J Pharm Sci. 2010 Jan–Feb; 72(1): 24–30.
3 Swarna SEM Uniformly arranged in agglomerates of size 1-
Makshika 2microns as compared to raw SM which
showed scattered arrangement of grains of
size 6-8micron
4 Swarna AAS 92% gold and no mercury
bhasma
3. Sudhaldev mahapatra ,C B Jha, Physicochemical Characterization of Ayurvedic bhasma
(Swarna makshika bhasma): An approach to standardization IJAR 2010;1(2)
4. Christopher L Brown, Gillian Bushell, Michael W Whitehouse, DS Agrawal,
SG Tupe, KM Paknikar, and Edward RT Tiekink, Characterization of the
gold in Swarna bhasma, a microparticulate used in traditional Indian medicine, Gold
Bulletin 2007 • 40/3
SUMMARY
• Various State of the art techniques are useful for
characterization of Rasoushadhies.
• For elemental scan in bulk-------EDAX,
• Elemental scan with conc -------------ICPMS
• for individual/trace elements-------------- AAS,
• for finer analysis of trace elements ---EPMA can be used.
• For particle size SEM or TEM can be used.
• For organic elucidation----------- FTIR
• Molecular structure ------------XRD
• ICP-MS: -Detects trace elements.
- With detection limits at or below the part per trillion (ppt)b range
- No other technology can provide the low detection limits and the
high productivity for elemental analysis offered by ICP-MS.
• SEM: Morphological and compositional information, a Scanning Electron
Microscope can detect and analyze surface fractures, provide information
in microstructures, examine surface contaminations, reveal spatial
variations in chemical compositions, provide qualitative chemical analyses
and identify crystalline structures.
• TEM: which give information about the size and shape of the micro-
structural constituents of the material. High-resolution image, that contains
information about the atomic structure of the material
• FTIR: The presence of particular functional group in a given organic
compound can be identified.