FOURIER TRANSFORM

INFRARED
SPECTROSCOPY(FTIR)
SPECTROSCOPY
Spectroscopy is the science of study the Interaction between radiation and matter.

The absorption of light, as it passes through a medium, varies linearly with the

distance the light travels and with concentration of the absorbing medium.

Where a is the absorbance, the Greek lower-case letter epsilon is a characteristic

constant for each material at a given wavelength (known as the extinction

coefficient or absorption coefficient), c is concentration, and l is the length of the

light path, the absorption of light may be expressed by the simple equation-

a= x c x l

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 Infrared radiation lies between the visible and microwave portions of the
electromagnetic spectrum.

Infrared waves have wavelengths longer than visible and shorter than microwaves,

and have frequencies which are lower than visible and higher than microwaves.

The Infrared region is divided into: near, mid and far-infrared.

Near-infrared refers to the part of the infrared spectrum that is closest to visible light

and far-infrared refers to the part that is closer to the microwave region.

Mid-infrared is the region between these two.

The primary source of infrared radiation is thermal radiation. (heat).

It is the radiation produced by the motion of atoms and molecules in an object. The

higher the temperature, the more the atoms and molecules move and the more
infrared radiation they produce.

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The INFRARED spectrum is divided into three region, which can be distinguished
each other by the Wavelength ranging from 14000 cm -1 to 20 cm-1.

Vibrational / Rotational

No. Region Range cm-1 Information

1 Near IR 14000 - 4000 Changes in Vibrational and rotational

levels, electron transitions

2 Mid-IR 4000 - 400 Changes in fundamental Vibrational levels

of most molecules

3 Far-IR 400 - 20 Rotational energy level changes

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TYPES OF INFRARED SPECTROPHOTOMETER
Dispersive Infrared Spectrophotometer

Fourier Transform Infra-Red SpectrophotometerCurrent technology (Fourier

Transform Infra-Red Spectroscopy, FTIR)

Dispersive IR FTIR
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PerkinElmer Model 297 PerkinElmer Spectrum 100
 A working
Instrument of
FTIR With a
Computer
connected to
it.

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INSTRUMENTATION

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Source-
Electronically Temperature Controlled (ETC) EverGlo.

The ETC EverGlo source is an efficient ceramic, refractory composite that

rapidly rises to operating temperature and is also thermally insulated to

maintain a constant operating temperature.

Provide energy for the spectral region from 7400 50 cm-1.

The source temperature is constantly monitored and controlled at 1140C

by the ETC.

Infrared energy is emitted from a glowing black-body source. This beam

passes through an aperture which controls the amount of energy presented

to the sample (and, ultimately, to the detector).
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LASER-
AHeliumneon laserorHe-Ne laser, is a type ofgas laserwhose gain

medium consists of a mixture of helium and neon (10:1) inside of a small

bore capillary tube, usually excited by a DC electrical discharge.

Laser create the drive volt for the moving mirror.

The He-Ne laser is used as an internal reference.

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Interferometer-
The beam enters the interferometer where the spectral encoding takes

place. The resulting interferogram signal then exits the interferometer.

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SCHEMATIC OF MICHELSON INTERFEROMETER

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SAMPLE-
The beam enters the sample compartment where it is transmitted through

or reflected off of the surface of the sample, depending on the type of

analysis being accomplished.

This is where specific frequencies of energy, which are uniquely

characteristic of the sample, are absorbed

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SAMPLE PREPARATION
IR Spectroscopy can be done on any pure sample regardless of the

physical state (solid, liquid, or gas).

However, we will only be discussing Sample Preparation for those samples

that are in the solid (2 methods) and liquid states (1 method).

The two common methods of Sample Preparation of pure solid are:

the KBr Pellet method,

the IR Polyethylene Card method.

The one common method of Sample Preparation using a pure liquid is:

the Solution Cell method.

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POLY ETHYLENE CARD METHOD-
1. Dissolve/Mix ~ 100 mg (0.1 g) of solid sample in ~ 2
mL of methylene chloride.

2. Add a drop or two of the mixture to one of the polyethylene

surface of the card.

3. Allow the methylene chloride to evaporate (~ 30

seconds) before putting into the IR machine.

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KBR PELLET METHOD-
1. Mix ~ 1 mg (0.001 g) of solid sample and ~ 100 mg
(0.1 g) of Potassium Bromide (KBr)
in the mortar.

2. Grind the contents in the mortar well with a pestle into a

fine mixture (~ 2 minutes).

3. Put a small amount of the finely crushed mixture into the

open chamber (2 piece metal), just enough to cover
the bottom surface of the
chamber.

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4. Put the lid on the chamber containing the finely
crushed mixture and put this 3 piece metal set
inside the Qwik Handi-Press, press hard and
then release the press.

5. Carefully take out the 3 piece metal from the Qwik

Handi-Press and the examine the Pellet formed within
the middle metal piece of the 3 piece metal set. The
Pellet should somewhat
clear and free from cracks.

6. If the pellet is opaque or has cracks, then we have to

redo the full procedure.

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7. Take the middle metal piece that has the somewhat
clear and uncracked pellet formed
and screw to the pellet holder.

8. This is the prepared sample by the KBr Pellet method in

which the IR can be determined.

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DETECTOR-
The beam finally passes to the detector for final measurement. The

detectors used are specially designed to measure the special interferogram

signal.

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 Fourier Transform Infrared Spectroscopy(FTIR)is a technique which is

used to obtain aninfraredspectrumofabsorptionoremissionof a solid,

liquid or gas.

FTIR Spectroscopy is a molecular spectroscopy which is used to

characterize both organic and inorganic evidence.

A method of obtaining an Infrared spectrum by measuring the

interferogram of a sample using an interferometer, then performing a
Fourier Transform upon the interferogram to obtain the spectrum.

The sample is bombarded with infrared radiation.

When the frequency of the infrared radiation matches the natural

frequency of the bond, the amplitude of the vibration increases, and the
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infrared is absorbed.
 The resulting spectrum represents the molecular absorption and transmission,

creating a molecular fingerprint of the sample.

Like a fingerprint, no two unique molecular structures produce the same infrared

spectrum. This makes infrared spectroscopy useful for several types of analysis.

The termFourier transform infrared spectroscopyoriginates from the fact that

aFourier transform(a mathematical process) is required to convert the raw data

into the actual spectrum.

The goal of anyabsorption spectroscopy(FTIR) is to measure how well a sample

absorbs light at each wavelength.

The output of an infrared spectrophotometer is a chart.

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 COMPARISON OF FT-IR & IR
Dispersive IR Fourier transform IR
1. There are many moving parts, 1. Only the mirror moves during the
resulting in mechanical slippage. experiment.
2. Calibration against reference 2. Use of laser provides high
spectra is required to measure frequency accuracy (to 0.01 cm-1).
frequency
3. Stray light causes spurious 3. Stray radiations do not affect the
readings. detector.

4. To improve resolution only a small 4. A much larger beam may be used

amount of IR beam is allowed to at all time. Data collection is easier.
pass.
5. Only radiation of a narrow 5. All frequency of radiation falls on
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frequency range falls on the detector the detector simultaneously.
ADVANTAGES OF FT-IR COMPARED TO DISPERSIVE IR

Short measurement time; all of the frequencies are measured simultaneously,

most measurements by FT-IR are made in a matter of seconds rather than several
minutes. This is sometimes referred to as the Felgett Advantage.

Throughput advantage (Jacquinot Advantage); advantage of FTIR is 100 times

better than a dispersive IR.

Measuring dark samples; Samples with high carbon content (such as black rubber)

can be measured.

Internally Calibrated; FTIR employ a He-Ne laser as an internal wavelength

calibration standard. He-Ne laser has a very stable frequency. Therefore, FTIR will
have excellent long term stability and repeatability in the spectrum. These
instruments Provides a precise measurement method which requires no external
calibration. 22
 Mechanical Simplicity: The moving mirror in the interferometer is the only

continuously moving part in the instrument. Thus, there is very little

possibility of mechanical breakdown.
Sensitivity; is dramatically improved with FT-IR for many reasons. The

detectors employed are much more sensitive, the optical throughput is

much higher. Sensitivity from very low parts per million to high percent
levels.
Simultaneous analysis of multiple gaseous compounds.

Measures a wide variety of volatile compounds (Inorganic and Organic).

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ADVANTAGES
FTIR is a simple and sensitive analytical tool.

Provide fast data acquisition & Simple to operate.

Most useful for analytical process.

To determine the composition of organic materials

To identify IR transparent or semi-transparent inorganic films

Provides quantitative determination of compounds in mixtures

Disadvantages
Interpretation of the data requires some experience.

Carbon di-oxide & Water Sensitive.

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APPLICATIONS OF FTIR
Identification of inorganic compounds and organic compounds.

Identification of components of an unknown mixture.

Analysis of solids, liquids, and gasses.

In measurement and analysis of Atmospheric Spectra.

Opaque or cloudy samples.

Energy limiting accessories such as diffuse reflectance or FT-IR

microscopes.

High resolution experiments (as high as 0.001 cm -1 resolution).

Trace analysis of raw materials or finished products.

Depth profiling and microscopic mapping of samples. 25