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Introduction to Fourier Transform Infrared Spectroscopy (FTIR)
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Introduction to
Fourier Transform
Infrared
Spectroscopy
(FTIR)
• Introduction to Fourier Transform Infrared Spectroscopy (FTIR)
❑ What is the FTIR?
Outline ❑ History of FTIR
• Principles of FTIR Spectroscopy
• Hook’s Law
• Infrared active bonds
• Classification of IR bands
• Instrumentation and Components of an FTIR Spectrometer
❑ Instrumentation FTIR Spectrometer
• Sample Preparation Techniques
• Advantages of FTIR Spectroscopy
• Applications of FTIR Spectroscopy
• Interpretation of FTIR Spectra
• Qualitative and Quantitative Analysis using FTIR
• Challenges and Limitations of FTIR Spectroscopy
• Future Trends and Developments in FTIR Technology
• References
Introduction to Fourier Transform Infrared
Spectroscopy (FTIR)
❑ What is the FTIR?
Fourier Transform Infrared Spectroscopy (FTIR) is a powerful analytical technique that
utilizes infrared radiation to identify and quantify molecular components in various
samples. FTIR spectroscopy is widely used in various fields, including chemistry,
biology, materials science, and environmental monitoring, for its versatility and ability
to provide detailed molecular information.
Infrared (IR) spectroscopy is one of the most used spectroscopic techniques in analytical laboratories for both qualitative and quantitative analysis. It
measures the interaction of IR radiation with a sample, to provide chemical identification. The three main areas studied by IR are the near-IR 14000-
4000 cm-1, mid-IR 4000-400 cm-1, and the far-IR 400-10 cm-1.
The mid-IR region is of most interest as it contains the characteristic bands for identification and is what is standardly regarded as IR spectroscopy. An
IR spectrometer measures the infrared light energy required to initiate molecular vibrations. The functional groups within molecules have unique
vibrational energies creating distinctive bands in the resulting IR spectrum that allow sample identification. Solids, liquids, and gasses can be analysed
using IR spectroscopy making it a highly versatile technique.
❑ History of FTIR
The first IR spectrometer was built in 1835, and it quickly became a valuable tool for
chemical characterisation. It was a dispersive design which means that the IR light is
split into its constituent frequencies (wavelengths) and each frequency detected
sequentially. The issue with this dispersive design was the long time it took to obtain
an entire spectrum due to the sequential detection. In the late 1960’s there was a
breakthrough for IR spectroscopy with the development of Fourier Transform Infrared
(FTIR) spectroscopy, which has now almost exclusively replaced dispersive
spectrometers. FTIR spectrometers measure all frequencies simultaneously resulting in
significantly faster acquisition times with improved signal to noise ratios and
wavenumber accuracy.
The basis of the FTIR spectrometer is the two beam interferometer originally designed
in 1891 by Michelson, Figure 2. It works by dividing a beam into two paths using a
beamsplitter, one beam is reflected by a fixed mirror and the second by a moving
mirror. They recombine at the beamsplitter after a path difference has been introduced
creating interference between the beams. Due to the changing travel distance of the
second beam, caused by the moving mirror, the resulting IR light has a varying
frequency distribution. The signal on the detector is recorded as a time-domain
interferogram which then undergoes a Fourier Transform to the frequency domain to
give the IR spectrum.
Principles of FTIR Spectroscopy
1 Infrared Radiation 2 Interferometer
Infrared radiation interacts with molecules causing molecular An interferometer splits the infrared beam into two paths, one
vibrations, including stretching and bending of bonds, which of which is delayed. The recombined beams create an
are specific to the molecular structure. This interaction is interference pattern that is unique to the sample. This
detected and analyzed in FTIR spectroscopy to provide interferogram is then mathematically transformed into a
information about the molecule's composition and functional spectrum, which displays the absorbance or transmittance of
groups present. the sample as a function of wavenumber (or frequency).
3 Spectral Interpretation 4 Fourier Transform
Each peak in the FTIR spectrum corresponds to a specific The interferogram, a time-domain signal, is mathematically
vibrational mode of the molecule. By analyzing the position, transformed into a frequency-domain spectrum using a
shape, and intensity of the peaks, one can identify the mathematical operation called the Fourier transform. This
functional groups present in the sample and obtain process allows us to obtain a spectrum with high resolution
quantitative information about their concentration. and sensitivity, providing detailed information about the
sample's molecular structure.
What is infrared absorption?
• In infrared spectroscopy, a sample is irradiated with infrared light,
and the transmitted or reflected light is measured, allowing
structural analysis and quantification. Absorbance analysis
involves measuring the amount of absorption of light by the
molecules in a sample, which is wavelength dependent. In the
case of ultraviolet and visible light (0.2 to 0.78 μm), absorption
occurs due to electronic transitions in molecules. In contrast,
infrared light (2.5 to 25 μm) is absorbed due to vibration and
rotation of molecules, and the energy involved is smaller.
Molecular vibrations and infrared absorption
In a molecule, interatomic chemical bonds can stretch as if they were springs. The energy
associated with such stretching vibrations is close to that of infrared light, so that molecules
absorb infrared light and vibrate. The vibrations that can be induced by infrared light are limited
to those involving a change in dipole moment. Infrared absorption does not occur if the
vibrations of bonds between atoms cancel each other. In the case of a linear molecule such as
CO2 , symmetric stretching vibrations do not absorb infrared light because the dipole moment
does not change, but asymmetric stretching vibrations do absorb infrared light because the
dipole moment changes. Atmospheric warming occurs because CO2 absorbs infrared light in this
manner, and so acts as a greenhouse gas.
In the case of H2O, which is a nonlinear molecule, both symmetric and asymmetric stretching
vibrations absorb infrared light because the dipole moment changes. The absorption band due to
symmetrical stretching appears at 3,652 cm-1, and that due to asymmetric stretching appears at
3,756 cm-1. In addition to stretching vibrations, infrared absorption also occurs for bending and
rotational vibrations, as long as the dipole moment changes.
Asymmetrical [Link]
Symmetrical [Link]
Stretching bonds
In plane deformation
1- Symmetrical stretching 2- Anti-symmetrical stretching
[Link]
Modo [Link]
Bending bonds
In plane deformation
Scissoring
[Link]
Rocking
[Link]
Bending bonds
Out of plane deformation
Wagging Twisting
Hooke's law
Hooke's Law states: that the vibrational frequency
is proportional to the strength of the spring; the
stronger the spring, the higher the frequency. the
vibrational frequency is inversely proportional to
the masses at the ends of the spring; the lighter the
weights, the higher the frequency.
❑ Increasing the atomic weight of the bonding atoms leads to shifting the absorption towards a high
wavelength according to Hooke's law.
❑ Increasing the bond strength causes the absorption to shift towards a higher wavenumber.
Infrared active bonds
The polarity of a bond has a significant impact on the intensity of an IR absorption band.
• Vibrations that cause a significant change in the dipole
moment of a chemical bond lead to strong absorption bands.
• Vibrations that result in no change/very little change in dipole
moment lead to very weak or no absorption band.
• Symmetrical bonds often exhibit very weak or no absorption band.
Classification of IR bands
IR bands can be classified as strong (s), medium (m), or weak (w), depending on their relative intensities
in the infrared spectrum. A strong band covers most of the y-axis. A medium band falls to about half of
the y-axis, and a weak band falls to about one third or less of the y-axis.
Instrumentation and Components of an FTIR
Spectrometer
Source Interferometer Detector
A source emits infrared radiation over a An interferometer splits the infrared The detector measures the intensity of
broad spectral range, typically a heated beam into two paths, one of which is the infrared radiation that passes
ceramic element or a globar. This source delayed. The recombined beams create through the sample. It is a sensitive
generates the infrared radiation that is an interference pattern that is unique to device that converts the incoming
used to interact with the sample. the sample. This interferogram is then infrared radiation into an electrical signal
mathematically transformed into a that can be processed by a computer.
spectrum, which displays the
absorbance or transmittance of the
sample as a function of wavenumber (or
frequency).
Instrumentation FTIR
Spectrometer
Hydraulic presses and other accessories for preparation of solid samples for
FTIR analysis.
Sample Preparation Techniques
Solid Samples Liquid Samples Gaseous Samples
Solid samples can be analyzed in Liquid samples are usually analyzed Gaseous samples are typically
various forms, including powders, using a liquid cell with appropriate analyzed using a gas cell with
films, fibers, or pellets. They can be path lengths. The choice of cell appropriate path lengths. The
directly analyzed using an attenuated depends on the sample's properties pressure and volume of the gas cell
total reflection (ATR) accessory or by and the desired analysis. need to be optimized for the analysis.
preparing a KBr pellet.
There are various measurement methods in FTIR spectroscopy, and these are
summarized below.
Transmission methods
Solid Methods
Gas method
Liquid Methods
1- KBr tablet method
2- Nujol method
1- Liquid-film method
3- KBr plate method
2- Solution method
4- Thin-film method
1- KBr tablet method
• This method is used for powder samples, and precise measurements can be
performed even with very small samples. However, due to the fact that KBr
absorbs moisture, it is not suitable when measuring samples whose spectra contain
absorption bands in the same regions as those due to water. Samples that contain
water, are highly hygroscopic, have a high concentration of carbon or pigments,
have an unstable crystal structure, or are relatively opaque to infrared light, are also
unsuitable. For chlorides and hydrochlorides, since a halogen exchange reaction
occurs between Br and Cl, sample pellets are generally produced using KCl.
• KBr pellets are easily prepared in minutes using an Evacuable Pellet Die. The
Press can be easily upgraded with Heated Platens in order to prepare polymer thin
films (when paired with the constant thickness film maker).
2- Nujol method
• A powder sample is mixed with liquid paraffin to form a
paste, which is then applied to the window plate. The Nujol
method is used for samples that are not suitable for the KBr
method, such as those that absorb moisture during sample
preparation (e.g., sugars), and samples that do not dissolve
in solvents (e.g., inorganic substances). It is also used for
reagents specified by official standards such as
pharmacopoeia, or for far-infrared measurements under a
N2 gas purge. However, this method is not suitable for
evaluating bands associated with CH groups (3,000 to 2,800,
1,500 to 1,300 cm-1) because of absorption by the liquid
paraffin in these wavenumber regions.
3- KBr plate
method
• This method uses crystalline KBr. A powder
sample is sandwiched between KBr plates and
measured. Since there is no need for crushing,
sample preparation is easy. It is an effective
method when simple sample preparation is
required, or for measuring highly hygroscopic
samples. However, samples that contain large
particles are susceptible to scattering of light,
so the measured absorbance may be lower than
the true value. This method cannot be used for
samples containing water.
4- Thin-film
method
• This method is for samples that can be
formed into thin films with a thickness of 10
μm or less. Various thinning methods can be
used, such as stretching, hot pressing, and
cutting. If the sample is soluble in a solvent,
the solution can be applied to an infrared
transmitting material (KBr plate), and
evaporating the solvent to form a thin film
becomes simple.
5- Liquid-film method
This method is suitable for samples of non-volatile liquids that have a high
viscosity, and also for qualitative analysis. The liquid is held between two
window plates in the assembled cell. Depending on the peak intensity, a
spacer may be needed to adjust the optical path length. For samples
containing water, a KBr window cannot be used.
6- Solution method
This method can be used to measure volatile solutions or to analyze the
concentration of trace additives dissolved in a solution. Before performing
the measurements, it is important to ensure that the solvent itself does not
give rise to absorption bands that interfere with those of the target
components
7- Gas method
• This method is used for gaseous samples.
The cell path length should be adjusted based
on the gas concentration. Since gaseous
samples usually produce sharp absorption
peaks, high-resolution measurements are
required. To determine the amount of water
vapor and carbon dioxide in a sample, use an
optical system that is under a full vacuum, or
perform a N2 gas purge to remove these
components completely.
There is a direct
method in modern undefined
FTIR devices.
FTIR Spectrometer
Advantages of FTIR Spectroscopy
1 Versatility 2 Sensitivity
FTIR can analyze a wide range of samples, including solids, FTIR is a sensitive technique that can detect and identify even
liquids, and gases, making it a highly versatile analytical trace amounts of compounds in a sample.
technique.
3 Specificity 4 Non-Destructive
FTIR provides detailed information about the molecular structure FTIR is a non-destructive technique, meaning it does not damage
of a sample, enabling the identification of specific functional or alter the sample during analysis, which is advantageous for
groups and the differentiation of similar compounds. analyzing valuable or delicate samples.
Applications of FTIR Spectroscopy
Chemistry Identification and quantification of
organic and inorganic compounds
Biology Analysis of biomolecules, such as
proteins, carbohydrates, and lipids
Materials Science Characterization of polymers,
composites, and other materials
Environmental Monitoring Analysis of air, water, and soil pollutants
Pharmaceutical Industry Quality control of drugs, analysis of drug
formulations, and identification of
impurities
Food Industry Analysis of food components, detection
of adulteration, and monitoring of food
quality
Interpretation of FTIR Spectra
1 Peak Identification
Identify the peaks in the spectrum and correlate them to specific vibrational
modes of the molecule.
2 Functional Group Analysis
Analyze the positions, shapes, and intensities of the peaks to identify the
functional groups present in the sample.
3 Peak Assignment
Assign the peaks to specific bonds or vibrations based on knowledge of the
molecular structure and comparison with spectral libraries.
4 Spectral Interpretation
Integrate the information obtained from peak identification, functional group
analysis, and peak assignment to draw conclusions about the sample's
composition and structure.
1
FTIR Spectra Examples
1- Organic compound (Benzene)
2- Inorganic Compound ( Graphite ) and nanomaterials (GO)
3- Ag NPs
3 2
•DOI: •DOI:
10.1088/2043-6254/aa84ec 10.1166/jnn.2018.14306
Qualitative and Quantitative Analysis using FTIR
Qualitative Analysis
Identify the components of a sample by comparing its spectrum to known spectra in databases or libraries. This involves
identifying the specific functional groups and the overall molecular structure of the compounds present.
Quantitative Analysis
Determine the amount of each component in the sample by measuring the intensity of specific peaks in the spectrum. This
often involves creating calibration curves or using standard methods for quantitative analysis.
Challenges and Limitations of FTIR Spectroscopy
Signal-to-Noise Ratio Spectral Overlap Water Interference Sample Preparation
Low signal-to-noise ratios can Multiple peaks may overlap, Water can significantly interfere Sample preparation techniques
hinder the detection of weak making it challenging to assign with the analysis of some samples can influence the obtained
signals, especially for trace and analyze all the peaks in the due to its strong infrared spectrum, and inconsistencies in
amounts of compounds. spectrum. absorption, especially in the sample preparation can lead to
region where many organic variations in the data.
molecules absorb.
Future Trends and Developments in
FTIR Technology
1 Miniaturization 2 Enhanced Sensitivity
Miniaturized FTIR spectrometers are Advanced detectors and signal
being developed for use in various processing techniques are being
applications, including handheld developed to improve the sensitivity of
devices for field analysis and point-of- FTIR spectroscopy, enabling the
care diagnostics. analysis of even smaller amounts of
samples.
3 Integration with Other 4 Data Analysis
Techniques Advanced data analysis techniques,
FTIR is being combined with other including chemometrics, are being
techniques, such as Raman developed to extract more information
spectroscopy, gas chromatography, and from FTIR spectra, enabling better
mass spectrometry, to provide more interpretation and identification of
comprehensive and complementary complex samples.
analytical information.
References
1- Pavia, D.L. (2001). Introduction To Spectroscopy 3ed.
2- JASCO Inc. (n.d.). Principles of infrared spectroscopy (5) Various measurement methods in FTIR spectroscopy -
Transmission methods - | JASCO Global. [online] Available at: [Link]
infrared-spectroscopy-5-various-measurement-methods-in-ftir-spectroscopy/.
3- [Link]. (2024). Liquid Samples. [online] Available at: [Link]
support/ftir/analysis_targets/[Link] [Accessed 3 Nov. 2024].
4- JASCO Inc. (n.d.). Principles of infrared spectroscopy (1) Molecular vibrations and infrared absorption | JASCO Global.
[online] Available at: [Link]
and-infrared-absorption/.
5- Master Organic Chemistry. (2016). IR Spectroscopy: 4 Practice Problems. [online] Available at:
[Link]
6- IRSpirit-X Series Fourier Transform Infrared Spectrophotometer
7- Shimadzu IRSpirit FTIR - Fourier Transform Infrared Spektrofotometre
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