ADVANCED MATERIAL CHARACTERISATION TOOLS & THEORIES

LECTURE 5:
FOURIER TRANSFORM
INFRARED SPECTROMETRY (FTIR)

PRESENTED BY
ASSOC. PROF. IR. TS. DR. MAHENDRAN SAMYKANO
 CONTENTS

• BASICS OF IR
• IR SPECTROSCOPY
• FTIR
• INSIGHTS OF FTIR
• ADVANTAGES, APPLICATIONS AND
DISADVANTAGES
 LEARNING OBJECTIVES
UPON THE CONCLUSION OF THIS LECTURE, YOU WILL HAVE ACQUIRED THE FOLLOWING PROFICIENCIES:

• ATTAIN A FUNDAMENTAL COMPREHENSION OF IR SPECTROSCOPY.

• FUNDAMENTAL KNOWLEDGE OF FOURIER TRANSFORMS.

• GAIN PROFOUND INSIGHTS INTO FTIR, COMPREHENDING ITS INTEGRAL COMPONENTS, FOUNDATIONAL PRINCIPLES, AND
OPERATIONAL MECHANISMS.

• ACQUIRE DEXTERITY IN THE METHODOLOGIES FOR PREPARING SAMPLES CUSTOMIZED FOR METICULOUS SCRUTINY
THROUGH FTIR ANALYSIS.

• EMBARK ON AN EXPLORATION OF THE EXAMINATION OF FTIR.

• INSIGHTS OF FTIR.
 FTIR

• lies between the visible and

microwave portions of the
electromagnetic spectrum.

• have wavelengths longer than

visible and shorter than microwaves
and have frequencies that are lower
than visible and higher than
microwaves.

• The primary source of infrared

radiation is thermal radiation.
(heat)
 WHAT IS INFRARED? (CONT.)
AT NORMAL BODY TEMPERATURE, HUMANS RADIATE MOST
STRONGLY IN THE INFRARED, AT A WAVELENGTH OF
ABOUT 10 MICRONS (A MICRON IS A TERM COMMONLY
USED IN ASTRONOMY FOR A MICROMETER OR ONE-
MILLIONTH OF A METER). IN THE IMAGE TO THE LEFT, THE
RED AREAS ARE THE WARMEST, FOLLOWED BY YELLOW,
GREEN AND BLUE (COOLEST).

The image to the right shows a cat in the infrared.

The yellow-white areas are the warmest and the
purple areas are the coldest. This image gives us a
different view of a familiar animal as well as
information that we could not get from a visible
light picture. Notice the cold nose and the heat from
the cat's eyes, mouth and ears.
 INFRARED SPECTROSCOPY

THE BONDS BETWEEN ATOMS IN THE MOLECULE STRETCH

AND BEND, ABSORBING INFRARED ENERGY AND
CREATING THE INFRARED SPECTRUM.

Symmetric Stretch Antisymmetric Stretch Bend

A molecule such as H2O will absorb infrared light when the

vibration (stretch or bend) results in a molecular dipole moment
change
 ENERGY LEVELS IN INFRARED
ABSORPTION

Excited
states
hn

Infrared Absorption and

Emission
h(n2 - n1)
n3
h(n1 - (overtone)
n2 h(n1 - n0)
n0 ) Ground
n1 (vibrational
n0 ) states

Infrared absorption occurs among the ground vibrational states, the energy differences,
and the corresponding spectrum, determined by the specific molecular vibration(s). The
infrared absorption is a net energy gain for the molecule and is recorded as an energy loss
for the analysis beam.
 INFRARED SPECTROSCOPY

A MOLECULE CAN BE CHARACTERIZED (IDENTIFIED) BY ITS MOLECULAR

VIBRATIONS BASED ON THE ABSORPTION AND INTENSITY OF SPECIFIC
INFRARED WAVELENGTHS.
 INFRARED SPECTROSCOPY
FOR ISOPROPYL ALCOHOL, CH(CH3)2OH, THE INFRARED ABSORPTION BANDS
IDENTIFY THE VARIOUS FUNCTIONAL GROUPS OF THE MOLECULE.
 CAPABILITIES OF INFRARED
ANALYSIS

 IDENTIFICATION AND QUANTITATION OF ORGANIC SOLID, LIQUID OR GAS

SAMPLES.
 ANALYSIS OF POWDERS, SOLIDS, GELS, EMULSIONS, PASTES, PURE LIQUIDS
AND SOLUTIONS, POLYMERS, PURE AND MIXED GASES.
 INFRARED USED FOR RESEARCH, METHODS DEVELOPMENT, QUALITY
CONTROL AND QUALITY ASSURANCE APPLICATIONS.
 SAMPLES RANGE IN SIZE FROM SINGLE FIBERS ONLY 20 MICRONS IN
LENGTH TO ATMOSPHERIC POLLUTION STUDIES INVOLVING LARGE AREAS.
 WHAT IS FT-IR?

 FT-IR STANDS FOR FOURIER TRANSFORM INFRARED, THE PREFERRED METHOD OF INFRARED
SPECTROSCOPY

 IN INFRARED SPECTROSCOPY, IR RADIATION IS PASSED THROUGH A SAMPLE

 THE SAMPLE ABSORBS SOME OF THE INFRARED RADIATION, AND SOME OF IT IS PASSED
THROUGH (TRANSMITTED)

 THE RESULTING SPECTRUM REPRESENTS THE MOLECULAR ABSORPTION AND TRANSMISSION,

CREATING A MOLECULAR FINGERPRINT OF THE SAMPLE
WHAT INFORMATION CAN FT-IR
PROVIDE?

It can identify unknown materials

It can determine the quality or consistency

of a sample

It can determine the number of

components in a mixture
 COMPARISON BETWEEN DISPERSION
SPECTROMETER AND FTIR
Dispersion
• In Spectrometer
order to measure an IR spectrum, the
dispersion Spectrometer takes several minutes.

• Also, the detector receives only a few % of the

energy of the original light source.

FTIR
• In order to measure an IR spectrum, FTIR
takes only a few seconds.

• Moreover, the detector receives up to 50% of

the energy of the original light source.

(much larger than the dispersion spectrometer.)

THE PRINCIPLES OF FTIR
METHOD
1. k is the force constant

2. μ is the reduced mass

3. Overtone Peaks

4. Dipole moment

5. Vibration modes
 IR LIGHT SOURCE

Intensity Distribution and Temperature Dependency versus Wavelength of Black Body Radiation
Energy
 FT OPTICAL SYSTEM
DIAGRAM
Light He-Ne gas laser
source

Beam splitter
Movable mirror

Sample chamber

Fixed mirror
Detector
Interferometer
HOW AN FTIR SPECTROMETER
WORKS?
CALIBRATION OF THE FTIR
SPECTROMETER
INTERFERENCE OF TWO BEAMS
OF LIGHT
INTERFERENCE IS A SUPER
POSITIONING OF WAVES
SAMPLING OF AN ACTUAL
INTERFEROGRAM

Interferometer interferogram

Output of a Laser interferometer

The primary interferometer interferogram that was sampled

Optical path difference x

FOURIER TRANSFORM
DETECTOR PROPERTIES

MCT
Operates at the temperatur
1010 of liquid nitrogen

D* (l, f) (cmHz1/2W-1)

109 TGS
Operates at room temperature

108
4000 600
Wavenumber[cm-1]
 SAMPLE PREPARATION
• THE SAMPLE PREPARATION METHOD DEPENDS ON THE TYPE OF MATERIAL
BEING ANALYZED.
• SOLIDS CAN BE GROUND INTO A FINE POWDER AND MIXED WITH
POTASSIUM BROMIDE (KBR) TO FORM A PELLET.
• LIQUIDS CAN BE DEPOSITED ON A SALT PLATE OR PLACED IN A LIQUID
CELL.
• GASES CAN BE PASSED THROUGH A GAS CELL.
 INSTRUMENTATION

• AN FTIR SPECTROMETER CONSISTS OF THE FOLLOWING

COMPONENTS:
• INFRARED SOURCE
• MICHELSON INTERFEROMETER
• SAMPLE COMPARTMENT
• DETECTOR
• COMPUTER
 ADVANTAGES

FELLGETT'S (MULTIPLEX) ADVANTAGE

• FT-IR COLLECTS ALL RESOLUTION ELEMENTS WITH A COMPLETE

SCAN OF THE INTERFEROMETER. SUCCESSIVE SCANS OF THE FT-IR
INSTRUMENT ARE COADDED AND AVERAGED TO ENHANCE THE
SIGNAL-TO-NOISE OF THE SPECTRUM.

• THEORETICALLY, AN INFINITELY LONG SCAN WOULD AVERAGE OUT

ALL THE NOISE IN THE BASELINE.

• THE DISPERSIVE INSTRUMENT COLLECTS DATA ONE WAVELENGTH AT

A TIME AND COLLECTS ONLY A SINGLE SPECTRUM. THERE IS NO
GOOD METHOD FOR INCREASING THE SIGNAL-TO-NOISE OF THE
DISPERSIVE SPECTRUM.
 CONNES ADVANTAGE
• AN FT-IR USES A HENE LASER AS AN INTERNAL
WAVELENGTH STANDARD. THE INFRARED
WAVELENGTHS ARE CALCULATED USING THE LASER
WAVELENGTH, ITSELF A VERY PRECISE AND
REPEATABLE 'STANDARD'.

• WAVELENGTH ASSIGNMENT FOR THE FT-IR SPECTRUM

IS VERY REPEATABLE AND REPRODUCIBLE AND DATA
CAN BE COMPARED TO DIGITAL LIBRARIES FOR
IDENTIFICATION PURPOSES.
 JACQUINOT ADVANTAGE
• FT-IR USES A COMBINATION OF CIRCULAR APERTURES AND
INTERFEROMETER TRAVEL TO DEFINE RESOLUTION. TO
IMPROVE SIGNAL-TO-NOISE, ONE COLLECTS MORE SCANS.

• MORE ENERGY IS AVAILABLE FOR THE NORMAL INFRARED

SCAN, AND VARIOUS ACCESSORIES CAN BE USED TO SOLVE
VARIOUS SAMPLE HANDLING PROBLEMS.

• THE DISPERSIVE INSTRUMENT USES A RECTANGULAR SLIT TO

CONTROL RESOLUTION AND CANNOT INCREASE THE SIGNAL-
TO-NOISE FOR HIGH-RESOLUTION SCANS. ACCESSORY USE IS
LIMITED FOR A DISPERSIVE INSTRUMENT.
 DISADVANTAGES

• SAMPLE PREPARATION CAN BE TIME-CONSUMING

• WATER VAPOR CAN INTERFERE WITH THE

SPECTRUM

• SOME SAMPLES ARE DIFFICULT TO ANALYZE

 APPLICATIONS

• IDENTIFICATION OF INORGANIC COMPOUNDS AND ORGANIC

COMPOUNDS
• IDENTIFICATION OF COMPONENTS OF AN UNKNOWN
MIXTURE
• ANALYSIS OF SOLIDS, LIQUIDS, AND GASSES
• IN REMOTE SENSING
• IN MEASUREMENT AND ANALYSIS OF ATMOSPHERIC SPECTRA
- SOLAR IRRADIANCE AT ANY POINT ON EARTH
- LONGWAVE/TERRESTRIAL RADIATION SPECTRA
• CAN ALSO BE USED ON SATELLITES TO PROBE SPACE
 ADDITIONAL INFO

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THANK YOU