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Department of chemistry

Assignment No – 01

Submitted To:

Dr Siraj -Ul-Haq

Submitted by:
Name Roll No
Hameeda Bibi 03
Bano Rasheed 06
Muhammad Atif 15
Sehreen Amin 17
Laiba Tajamal Awan 19
Shiza Mehrban 28
Momina Munsaf 32
Muneeba Majeed 40

Course Title:

Special topic in Inorganic Chemistry

Course Code:

CHM-722 Class:

MPhil 1st

Topic: Fourier Transform Infrared Spectroscopy

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Table of contents:
• Introduction
• History
• Instrumentation
• Principle
• Working
• Advantage & Disadvantage

 Introduction:

Infrared (IR) spectroscopy encompasses various techniques for analyzing how molecules interact
with infrared light. The two primary methods are Dispersive Infrared (IR) Spectroscopy and
Fourier Transform Infrared (FTIR) Spectroscopy.

Dispersive Infrared (IR) Spectroscopy:

This traditional method employs a monochromator, such as a prism or diffraction grating, to disperse
the infrared light into its component wavelengths. The instrument sequentially measures the intensity
of each wavelength passing through the sample, producing the IR spectrum. While effective, this
approach can be time-consuming due to the sequential nature of the measurements and may have a
lower signal-to-noise ratio compared to FTIR.

Fourier Transform Infrared (FTIR) Spectroscopy:

FTIR is a more advanced technique that collects all wavelengths simultaneously. It utilizes an
interferometer to modulate the infrared light, generating an interferogram—a signal containing all the
spectral information. A mathematical process called Fourier transform is then applied to convert this
interferogram into the conventional IR spectrum. FTIR offers several advantages over dispersive
methods, including faster data acquisition, improved sensitivity, and a higher signal-to-noise ratio.

Key Differences Between Dispersive IR and FTIR Spectroscopy:

• Data Acquisition: Dispersive IR measures one wavelength at a time, whereas FTIR captures
all wavelengths simultaneously.
• Speed: FTIR is generally faster due to its simultaneous data collection.
• Sensitivity: FTIR typically provides a higher signal-to-noise ratio, enhancing its sensitivity.
• Instrumentation: Dispersive IR relies on prisms or gratings for wavelength dispersion, while
FTIR uses an interferometer coupled with a Fourier transform for spectrum generation.

In modern analytical applications, FTIR has largely supplanted dispersive IR spectroscopy due to
these advantages. However, the choice between the two methods may depend on specific analytical
requirements and available instrumentation.
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✓ Fourier Transform Infrared Spectroscopy (FTIR) analytical technique used for

identifying and characterizing the chemical composition and molecular
structure of materials.
✓ FTIR is widely used in nanotechnology for analyzing the chemical
composition, bonding, and surface properties of nanomaterials. It helps
researchers understand how functional groups interact at the nanoscale.
History of Fourier Transform Infrared Spectroscopy (FTIR)
o FTIR spectrometry was developed inorder to overcome the limitations encountered
with dispersive instrument .
o The scientific idea behind the Fourier-transform infrared (FT-IR) spectroscopy was
first initiated in the late 1880s by Albert A. Michelson.

 Instrumentation of Fourier Transform Infrared Spectroscopy (FTIR)

This is a diagram of the instrumentation used in Fourier Transform Infrared (FTIR)

spectroscopy.
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Light Source:

4,000 to 400 cm−1 is a range of values that can be used in Fourier Transform
Infrared (FTIR) spectroscopy. FTIR is a non-destructive analytical technique that uses
infrared light to characterize materials.

In Fourier Transform Infrared (FTIR) spectroscopy, the choice of radiation

source is crucial for obtaining accurate and reliable spectra. The most
commonly used sources in FTIR instruments include:

1. Globar (Silicon Carbide Source): A Globar is a silicon carbide rod that is

electrically heated to high temperatures, typically around 1300 K, emitting a
broad spectrum of mid-infrared radiation. It is widely used due to its stability
and broad spectral output.

2. Nernst Glower: Composed of rare earth oxides, a Nernst glower becomes

electrically conductive and emits infrared radiation when heated. However, it
requires a preheating phase to become conductive and is less commonly
used in modern instruments.

3. Quartz Tungsten-Halogen Lamp: This source is typically used for near-

infrared applications, emitting radiation in the near-IR region. It consists of a
tungsten filament enclosed in a quartz envelope filled with a halogen
gas.Provides infrared (IR) radiation that passes through the interferometer.

1. Interferometer:

Central component of the FTIR system that modulates the IR radiation to create an interference
pattern. It consists of:
Beam Splitter: Divides the incoming light into two beams.

Movable Mirror: Creates path length differences by moving, which causes variations in the
interference pattern.

Fixed Mirror: Reflects the beam back toward the beam splitter.

2. He-Ne Gas Laser:

Provides a reference laser beam to ensure precise measurements of the mirror's movement in
the interferometer.

3. Sample Chamber:
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The modulated IR beam passes through the sample in this chamber. The sample absorbs specific
frequencies of IR radiation corresponding to its molecular vibrations.

4. Detector:

Measures the intensity of the transmitted or reflected IR beam after it interacts with the sample.
The detector converts the signal into data that can be processed.

✓ The magnification range of FTIR spectroscopy is typically expressed in wavenumbers,

and is generally considered to be between 4000 cm⁻¹ and 400 cm⁻¹. This means that
FTIR can detect and analyze infrared radiation within this specific range of frequencies,
providing a detailed "fingerprint" of a molecule based on its vibrational modes.
✓ Resolution in FTIR spectroscopy refers to the ability to distinguish between
closely spaced peaks in the spectrum
✓ The resolution can be set to values such as 16 cm-1, 8 cm-1, 4 cm-1, or 2 cm-1

❖ Principle of FTIR
When a molecule is exposed to infrared radiation, the energy causes the bonds within the
molecule to vibrate (stretching, bending, etc.). Each type of bond absorbs infrared light at a
specific wavelength, creating a unique absorption pattern or "fingerprint."
FTIR differs from traditional dispersive IR spectroscopy by using a Fourier Transform to
convert the raw data collected by the spectrometer (interferogram) into an interpretable
infrared spectrum.
Sample preparation
Sample Preparation for FTIR Analysis of Nanoparticles
Proper sample preparation is essential for accurate FTIR analysis of
nanoparticles. The method used depends on the nanoparticle type (solid,
liquid, or film). Here are the main techniques:
1. KBr Pellet Method (For Solid Nanoparticles)
Best for: Powdered nanoparticles (e.g., metal oxides, carbon-based NPs).
Why use it? Provides clear transmission spectra with minimal background
interference.
Procedure:
1. Weigh 1-2 mg of the nanoparticle powder.
2. Mix with 100 mg of dry KBr powder (acts as a transparent matrix).
3. Grind the mixture finely using a mortar and pestle.
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4. Press the powder into a thin, transparent pellet using a hydraulic press (~10
tons pressure).
5. Place the pellet in the FTIR spectrometer and record the spectrum.

Precautions:
KBr is hygroscopic; avoid moisture contamination.
Ensure nanoparticles are evenly dispersed in KBr for accurate results.
2. ATR (Attenuated Total Reflectance) Method (For Liquid & Surface-Coated
Nanoparticles)
Best for: Liquid suspensions, surface-functionalized nanoparticles, or thin
coatings.
Why use it? No need for KBr pellets; allows direct measurement of
nanoparticle surfaces.
Procedure:
1. Place a small drop of nanoparticle suspension (or a thin layer of powder)
on the ATR crystal (ZnSe, Ge, or diamond).
2. Apply pressure to ensure contact between nanoparticles and the ATR
crystal.
3. Run the FTIR scan and collect the spectrum.
Advantages:
Minimal sample preparation (no grinding or pressing needed).
Suitable for hydrocolloidal nanoparticles (gold, silver, TiO₂, ZnO, etc.).
3. Thin Film Method (For Nanoparticle Coatings & Nanocomposites)
Best for: Polymer-nanoparticle composites, nanoparticle coatings, or
functionalized surfaces.
Why use it? Ideal for studying surface modifications and nanoparticle-
polymer interactions.
Procedure:
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1. Dissolve nanoparticles in a volatile solvent (e.g., ethanol, chloroform).

2. Drop-cast or spin-coat the solution onto a clean glass or silicon substrate.
3. Allow the solvent to evaporate, leaving behind a thin nanoparticle film.
4. Place the substrate directly in the FTIR spectrometer and scan.
Applications:
Analyzing surface-functionalized nanoparticles (e.g., thiol-coated gold NPs).
Studying nanoparticle-polymer interactions in coatings.
4. Diffuse Reflectance (DRIFT) Method (For Highly Absorptive
Nanoparticles)
Best for: Nanoparticles with strong IR absorption (e.g., carbon-based
materials).
Why use it? Avoids intense absorption that can obscure spectral peaks.
Procedure:
1. Mix nanoparticles with KBr (or other IR-transparent powders).
2. Place the mixture in a DRIFT sample holder.
3. Collect the reflectance spectrum, which is then converted to an absorption
spectrum.
Used for:
Carbon nanotubes (CNTs), graphene oxide (GO), fullerenes.
Highly absorbing metal nanoparticles (Fe₃O₄, TiO₂, etc.).
❖ Working of Fourier Transform Infrared spectroscopy
The working principle of FTIR (Fourier Transform Infrared) spectroscopy relies on the
interaction of infrared radiation with a sample to identify its molecular composition.
Here’s how the system works step-by-step:
1. Infrared Light Emission:
The IR light source emits infrared radiation, which is directed toward the interferometer.
2. Beam Splitting in the Interferometer:
In the interferometer, a beam splitter divides the IR light into two paths:
• One beam travels to a fixed mirror.
• The other beam travels to a movable mirror.
Both beams are reflected back to the beam splitter, where they recombine. Because the
movable mirror changes its position, it creates a difference in the path lengths of the two
beams, leading to an interference pattern.
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3. Formation of Interference Pattern:

The interference pattern depends on the relative path difference between the two beams.
This pattern contains information about the entire IR spectrum of the light source.
4. Passing through the Sample:
The recombined beam passes through the sample in the sample chamber.
Molecules in the sample absorb specific frequencies of the IR radiation based on their
vibrational modes (such as stretching, bending, or twisting of chemical bonds).
5. Detection:
The remaining IR radiation that is not absorbed by the sample reaches the detector. The
detector measures the intensity of the transmitted light as a function of the mirror
position, recording an interferogram.
6. Fourier Transform:
The recorded interferogram (time-domain signal) is mathematically converted using a Fourier
Transform to produce a spectrum in the frequency domain.
The output spectrum shows the intensity of absorbed light as a function of wavelength or
wavenumber, representing the molecular "fingerprint" of the sample.
7. Analysis:
The IR spectrum shows peaks at specific wavenumbers, corresponding to the vibrational
frequencies of bonds in the sample. Each compound has a unique IR spectrum, allowing for:
Identification of functional groups.
Qualitative and quantitative analysis of chemical composition.

❖ FTIR Analysis of ZnO-Based Nanomaterials

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➢ This FTIR (Fourier Transform Infrared) spectrum provides important insights into the
functional groups present in a nanomaterial, particularly one that contains zinc oxide
(ZnO) nanoparticles.
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Key Peaks and Their Assignments:
1. 3438 cm⁻¹ (O-H Stretching)
Indicates the presence of hydroxyl (-OH) groups.
In nanotechnology, hydroxyl groups enhance surface functionalization, improving dispersion and
biocompatibility in biomedical applications.
2. 2918 cm⁻¹ (C-H Stretching)
Suggests the presence of aliphatic hydrocarbon chains.
This could indicate organic coatings or surfactants used to stabilize ZnO nanoparticles, preventing
aggregation in nanocomposite formulations.
3. 2367 cm⁻¹ (C-O Stretching)
Associated with carbonyl (-C=O) or carbonate (-CO₃) functional groups.
This may be due to organic modifications or atmospheric CO₂ adsorption on the ZnO nanoparticle
surface.
4. 1634 cm⁻¹ & 1446 cm⁻¹ (C=C Stretching)

Suggests the presence of conjugated C=C bonds, possibly from graphene, carbon nanostructures, or
aromatic organic compounds.
This is significant in nanotechnology, where ZnO-graphene nanocomposites are used in electronics,
catalysis, and energy storage.
5. 1033 cm⁻¹, 876 cm⁻¹, 701 cm⁻¹ (Zn-O Stretching)
These peaks confirm the presence of zinc oxide (ZnO) nanoparticles.
ZnO nanoparticles have wide applications in optoelectronics, sensors, drug delivery, and antimicrobial
coatings.
Advantages of FTIR Spectroscopy:

Advantages of FTIR in Nanotechnology

Fourier Transform Infrared (FTIR) Spectroscopy is a powerful tool in nanotechnology for

characterizing nanomaterials. It provides valuable insights into the chemical composition, functional
groups, and surface modifications of nanostructures.

1. Identification of Functional Groups

• FTIR helps detect functional groups (-OH, -COOH, -NH₂, etc.) present on nanomaterial surfaces.
• This is crucial for surface functionalization, which enhances properties like dispersion,
biocompatibility, and reactivity.

2. Confirmation of Nanoparticle Synthesis

• FTIR is used to confirm the successful synthesis of metal oxide nanoparticles (e.g., ZnO, TiO₂, Fe₂O₃)
by identifying characteristic metal-oxygen (M-O) bonds.
• Ensures the purity and chemical composition of nanoparticles.
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3. Surface Modification and Coating Analysis

• Many nanomaterials are coated with polymers, surfactants, or biomolecules to improve stability and
functionality.
• FTIR detects the presence of these coatings, ensuring effective drug delivery systems, biosensors,
and catalysts.

4. Rapid and Non-Destructive Analysis

FTIR allows quick analysis without altering the nanomaterial structure. This is important for quality
control in nanotechnology applications like electronics, medical devices, and coatings..

5. Interaction Studies in Nanocomposites

FTIR can analyze interactions between nanoparticles and other materials (e.g., ZnO-graphene, TiO₂-
polymer composites).

Helps optimize nanocomposite materials for energy storage, flexible electronics, and environmental
applications.

6. Detection of Contaminants and Impurities

FTIR can identify unwanted organic or inorganic impurities in nanoparticle synthesis.

Ensures high-quality nanomaterials for biomedical, pharmaceutical, and industrial applications.

Disadvantages of FTIR (Fourier Transform Infrared Spectroscopy)

FTIR is a widely used analytical technique, but it has certain limitations, especially in
nanotechnology and material characterization. Below are some key disadvantages:

1. Limited Detection of Inorganic Compounds

• FTIR is more effective for identifying organic molecules and is less suitable for detecting inorganic and
metallic compounds that do not exhibit strong IR absorption (e.g., metals, metal alloys).
• Some nanomaterials, like pure metals (Au, Ag, Cu) or carbon-based materials (graphene, CNTs), have
weak IR signals.

2. Low Sensitivity for Low-Concentration Samples

• FTIR may not effectively detect very low concentrations of nanoparticles or thin surface coatings due
to weak absorbance signals.
• This can be a challenge in nanotechnology, where detecting trace modifications on nanomaterial
surfaces is crucial.
• 3. Overlapping Peaks and Complex Spectra

• Functional groups with similar absorption frequencies can lead to overlapping peaks, making it
difficult to differentiate between chemical species.
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• This can be problematic in nanocomposites, where multiple materials contribute to the spectrum.

4. Sample Preparation Limitations

• Solid samples require special preparation (e.g., pelletizing with KBr or using ATR mode), which may
alter their structure.
• Water interference: FTIR is highly sensitive to water, which can mask important peaks in hydrated
samples or biological nanomaterials.

5. Limited Quantitative Analysis

While FTIR provides qualitative data about functional groups, it is less accurate for precise
quantitative measurements compared to other techniques like UV-Vis or mass spectrometry.

6. Surface vs. Bulk Analysis Limitation

• FTIR mostly analyzes surface functional groups and may not provide detailed information about the
bulk composition of nanoparticles.
• Techniques like X-ray diffraction (XRD) or Transmission Electron Microscopy (TEM) are often needed
for full material characterization.

❖ Conclusion:
FTIR spectroscopy is a versatile and powerful analytical technique widely used in material
identification, qualitative and quantitative analysis, and molecular structure determination.
Its advantages, such as high sensitivity, speed, and non-destructive nature, make it a
preferred method in industries like pharmaceuticals, environmental science, and polymers.
However, FTIR has limitations, such as its inability to analyze IR-inactive molecules and the
need for careful sample preparation. Despite these drawbacks, FTIR remains an essential tool
for analyzing organic and inorganic compounds due to its accuracy, broad applicability, and
ability to provide unique molecular "fingerprints." With advancements in technology, FTIR
continues to evolve, becoming even more user-friendly and efficient for a wide range of
applications.

References:

➢ Pavia, D. L., Lampman, G. M., Kriz, G. S., & Vyvyan, J. R. (2014). Introduction
to Spectroscopy .
➢ https://www.researchgate.net/figure/FTIR-spectra-of-ZnO-
nanoparticles_fig1_363380465
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