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C5 IR Spectros

This document discusses infrared spectroscopy, including: 1. Infrared spectroscopy measures molecular vibrations to extract structural information about molecules and provide molecular fingerprints for characterization and identification. 2. Infrared instrumentation includes sources like tungsten filament lamps, monochromators using prisms or gratings to separate wavelengths, and detectors like thermocouples, bolometers, and photoconductive cells that convert infrared radiation to electrical signals. 3. Samples can be prepared as gases in cells, liquids in sealed cells or sandwiched between plates, and solids as thin films, in mulls mixed with oil, or as pressed pellets mixed with KBr.

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564 views13 pages

C5 IR Spectros

This document discusses infrared spectroscopy, including: 1. Infrared spectroscopy measures molecular vibrations to extract structural information about molecules and provide molecular fingerprints for characterization and identification. 2. Infrared instrumentation includes sources like tungsten filament lamps, monochromators using prisms or gratings to separate wavelengths, and detectors like thermocouples, bolometers, and photoconductive cells that convert infrared radiation to electrical signals. 3. Samples can be prepared as gases in cells, liquids in sealed cells or sandwiched between plates, and solids as thin films, in mulls mixed with oil, or as pressed pellets mixed with KBr.

Uploaded by

surya
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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Chapter 5 – Materials Characterization – IR Spectroscopy

Infrared Spectroscopy

1
Chapter 5 – Materials Characterization – IR Spectroscopy

Infrared Spectroscopy

• Energy absorption by molecule in infrared region


• Transition between two vibrational levels
• Extract molecular structural information by measuring molecular
vibrations spectra
• Molecular fingerprints, characterize and identify the molecule
• Used in conjunction with Raman Spectroscopy
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation

• Dispersive – prism or grating


• Non-dispersive – interference filters, tunable lasers sources, an
interferometer (Fourier Transform Infrared Spectrometer
• For IR region, front faced mirrors
• Glass and quartz absorb opaque to IR
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


1. Source of Infrared radiation
• IR, heat radiation
• Heat transfer direct, do not require a direct physical medium
• Converted to heat, only on absorption by object
• Source, an incandescent solid material which has a radiant energy
distribution
• Similar to theoretical black body
• Tungsten filament lamp, Glober, Nernst Glower, Nichrome heater
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


2. Infrared monochromator
• Means of separating source radiation wavelengths
• Prisms and gratings
• Prisms of alkali halides
• Large crystals, Prisms, windows and cells are cut from them
• NaCl 4000-650 cm-1
• Potassium bromide 1000-400 cm-1
• Cesium iodide 1000-260 cm-1
• Below 250 cm-1, gratings are used, disperse the energy
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


3. Infrared Detector
• Thermal radiant energy into electrical energy
• Selective – response dependent on wavelength incident radiation
• Photographic plates, photocells, photoconductive cells, infrared
phosphors
• Photoconductive important, rapid response and high sensitivity
• PbS, PbSe, Lead telluride, selenium
• Increase in conductivity, with increase in IR illumination
• 0.5 – 3.5 microns
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


3. Infrared Detector
• Non-selective – response independent of wavelength of incident
radiation
• Directly proportional to incident energy
• Thermocouples, bolometers, pneumatic cell
• Thermocouples: evaporating bismuth antimony, semiconductor
alloys, on thin film cellulose nitrate, in evacuated chamber with KBr
window
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


3. Infrared Detector
• Bolometer: Electrical signal, change in resistance of a metallic
conductor with temperature
• Faster response time due to small thermal capacity
• Thermistor bolometer, increased sensitivity
• Fused mixture of metal oxides : Ni, Co, Mn, exponential decrease in
resistance with temperature
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


3. Infrared Detector
• Pneumatic detector cell : Two cells, first 3 mm filled with a gas (Xe),
connected to second cell through a tube
• One end closed with a curved diaphragm, acting as mirror
• Heat on gas changes the volume, expansion due to IR absorption
• Thereby moving mirror in other cell proportionally
Chapter 5 – Materials Characterization - IR Spectroscopy

Preparation of samples
1. Gaseous samples
• No special preparation
• 10 cm long cell for gaseous samples
• Vacuum tight cells
• Connection problems
• Proper operation, due to heating and cooling cycles
Chapter 5 – Materials Characterization - IR Spectroscopy

Preparation of samples
2. Liquid or solution samples
• Pure liquid samples
• No solvents, as they have their own absorption spectra
• Liquid and solution, same type of cell
• Non-corrosive and not too viscous liquids, normally in sealed cells
• Highly viscous liquids, sandwiched as a layer between two salt
plates
• Cavity cells
Chapter 5 – Materials Characterization - IR Spectroscopy

Preparation of samples
3. Solids
• Solid Films: solid samples into thin films, on IR transmitting
window, or solid melted and cooled into thin film, not
recommended for crystalline substances
• Mull-Technique: Powdered sample mixed with a little heavy
paraffin oil, nujol, mulled into paste, transferred to rock salt plate
• Pressed Pellet Technique: Weighed solid material thoroughly mixed
with KBr, pressed into pellet under high pressure in evacuated die,
resulting in transparent discs
Chapter 5 – Materials Characterization – IR Spectroscopy

13

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