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This document is an assignment on Fourier Transform Infrared Spectroscopy (FT-IR) for a BS 3rd Year Analytical Chemistry course. It covers fundamental concepts, principles, instrumentation, and applications of FT-IR, including the types of samples that can be analyzed and the significance of various components like the Michelson interferometer and beam splitter. Additionally, it explains how FT-IR detects functional groups, the importance of baseline correction, and the interpretation of FT-IR spectra.

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0% found this document useful (0 votes)
57 views18 pages

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This document is an assignment on Fourier Transform Infrared Spectroscopy (FT-IR) for a BS 3rd Year Analytical Chemistry course. It covers fundamental concepts, principles, instrumentation, and applications of FT-IR, including the types of samples that can be analyzed and the significance of various components like the Michelson interferometer and beam splitter. Additionally, it explains how FT-IR detects functional groups, the importance of baseline correction, and the interpretation of FT-IR spectra.

Uploaded by

bakhtawer mari
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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NAME IQRA ZAI

ROLL NO: BSCHM-2022-043


BS 3rd Year
Semester-VI
ANALYTICAL CHEMISTRY ASSIGNMENT
ASSIGNED BY:
Ms.Aysha Rajput

General Questions:
Q: What is FT-IR spectroscopy?
• Answer : Fourier Transform Infrared Spectroscopy, also known as
FTIR Analysis or FTIR Spectroscopy, is an analytical technique used to
identify organic, polymeric, and, in some cases, inorganic materials. The
FTIR analysis method uses infrared light to scan test samples and observe
chemical properties.

Q: What does FT-IR stand for?


• Answer : ( FT-IR stand for Fourier) Transform Infrared
Spectroscopy .

Q: What is the principle of FT-IR spectroscopy?


Answer : FTIR, or Fourier Transform Infrared Spectroscopy, is a technique
used to obtain the infrared spectrum of absorption or emission of a solid, liquid,
or gas. The principle of FTIR is based on the interaction of infrared radiation
with molecular vibrations.
When infrared light passes through a sample, certain wavelengths of the light
are absorbed by the molecules in the sample. This absorption occurs because
the energy of the infrared light matches the energy required to excite specific
molecular vibrations, such as stretching or bending of chemical bonds.
• Each type of bond and molecular structure has unique vibrational frequency,
which corresponds to specific wavelengths of infrared light. As a result,
when a sample is exposed to infrared radiation, it will absorb light at
characteristic wavelengths, creating a spectrum that acts like a molecular
fingerprint.

Q: What is the purpose of FT-IR analysis?


• Answer : The purpose of FT-IR (Fourier Transform Infrared)
analysis is to identify and characterize unknown materials by analyzing their
chemical composition based on the vibrational frequencies of their
molecular bonds, allowing researchers to determine the presence of specific
functional groups within a molecule and thus identify the compound itself,
as well as potentially quantify its concentration within a sample; essentially,
it provides detailed information about the molecular structure of a substance
by measuring how much infrared radiation it absorbs at different
wavelengths.

Q: What type of samples can be analyzed using FT-IR?


Types of Samples for FTIR Analysis
• FTIR spectroscopy can analyze a wide range of sample types, including
solids, liquids, and gases.

1. Solid Samples:

• Pellets: Solid samples can be ground with potassium bromide (KBr) and
pressed into a thin pellet. This method is commonly used for inorganic
compounds.
• Thin Films: Solids can be dissolved in a suitable solvent and cast onto an
infrared-transparent substrate to form a thin film. Polymers and organic
materials are often analyzed this way.
• Powders: Fine powders can be analyzed using an attenuated total
reflectance (ATR) accessory, which allows direct measurement without
extensive preparation.
• Fibers and Fabrics: These materials can be examined using ATR or by
creating thin sections that can be analyzed using transmission FTIR.

2. Liquid Samples:

• Neat Liquids: Pure liquids can be placed directly in the path of the
infrared beam using liquid cells with appropriate window materials (e.g.,
NaCl or KBr windows).
• Solutions: Liquids can be analyzed in solution form. The solvent
should be chosen such that it does not interfere with the IR spectrum of the
analyte.
• Droplet on ATR: A small droplet of the liquid sample can be placed
on the ATR crystal for direct analysis.

3. Gas Samples:

• Gas Cells: Gases are typically analyzed using gas cells with long
path lengths to increase sensitivity. The cell windows must be transparent to
infrared light, commonly made from materials like CaF2 or KBr.

Instrumentation Questions:
Q: What are the main components of an FT-IR spectrometer?
The Components of FTIR Spectrometers
A common FTIR spectrometer consists of a source, interferometer, sample
compartment, detector, amplifier.
SOURCE of radiation in FT-IR: Generally we can use GLOBAR SOURCE,
NERNST GLOWER .These two sources are useful in the mid IR region which
is from 4000 and 400cm-1
TUNSTEN-HALOGEN LAMP for near IR region
For far IR region use high pressure MERCURY VAPOUR LAMP .So these are
the sources can use in order to produce IR radiation.
INTERFEROMETER: In FT-IR spectroscopy MICHELSON interferometer
is used.
Michelson interferometer is consists of three parts
1.A Beam splitter at 45 angle that divides radiations Into two beams .
2. Stationary/ fixed mirror
3. Moving mirror
SAMPLE HOLDER SAMPLE HOLDER : Is typically made up of salts
Which is not absorbed IR radiation . such as KBR(Potassium bromide) , NaCl
(Sodium chloride) , CaF2(Calcium fluoride),ZnSe (zinc selenide)
DETECTORs : There are three types of detectors used in FT-IR instrument .
1.Thermocouples 2.Pyroelectric detector 3. Photoelectric detector but in this we
use thermocouples.

Q: How does the interferometer work in FT-IR?


Answer: A typical Michelson interferometer consists of two perpendicular
mirrors and a beamsplitter. One of the mirror is a stationary mirror and another
one is a movable mirror. The beamsplitter is designed to transmit half of the
light and reflect half of the light. Subsequently, the transmitted light and the
reflected light strike the stationary mirror and the movable mirror, respectively.
When reflected back by the mirrors, two beams of light recombine with each
other at the beamsplitter.

If the distances travelled by two beams are the same which means the
distances between two mirrors and the beamsplitter are the same, the
situation is defined as zero path difference (ZPD). But imagine if the
movable mirror moves away from the beamsplitter, the light beam which
strikes the movable mirror will travel a longer distance than the light beam
which strikes the stationary mirror. The distance which the movable mirror
is away from the ZPD is defined as the mirror displacement and is
represented by ∆. It is obvious that the extra distance travelled by the light
which strikes the movable mirror is 2∆. The extra distance is defined as the
optical path difference (OPD) and is represented by delta. Therefore,
• δ=2Δ
• It is well established that when OPD is the multiples of the
wavelength, constructive interference occurs because crests overlap with
crests, troughs with troughs. As a result, a maximum intensity signal is
observed by the detector. This situation can be described by the following
equation:
• δ=nλ
• with n = 0,1,2,3...
• In contrast, when OPD is the half wavelength or half wavelength add
multiples of wavelength, destructive interference occurs because crests
overlap with troughs. Consequently, a minimum intensity signal is observed
by the detector. This situation can be described by the following equation:
1
• δ=(n+2) λ
• with n = 0,1,2,3...

Q: What is a Michelson interferometer, and why is it used in FT-
IR?
Answer: A Michelson interferometer is an instrument in which the
phenomena of interference is used to make precise measurements of
wavelengths refractive index and distance . An FTIR spectrometer uses a
Michelson interferometer . it is used to split one beam of light into two so
that the paths of the two beams are different results in constructive and
destructive interference based on the relative positions of a stationary and
moving mirror.

Q: What is the role of the beam splitter in FT-IR?


• Answer: A Beam splitter is present in interferometer at 45 angle that
divides radiations Into two beams .
• 1. Division of IR Radiation: The beam splitter divides the IR
radiation from the source into two perpendicular beams.
• 2. Creation of Interference Pattern: The beam splitter recombines the
two beams, creating an interference pattern that is measured by the detector.
Q: How is an infrared source different from a visible light source?
• Wavelength: Infrared radiation has a higher wavelength than visible light.
• Perception: Humans cannot see infrared light.
• Heat generation: Infrared sources often produce less heat compared to visible
light sources.
• ENERGY: visible light has higher energy than infrared light
Examples:
• Visible light source: an visible light can be obtained by incandescent lamp with
tungsten filament
• Infrared light source: an IR radiations can be obtained by Nernst glower, globar
etc

Q: What is an interferogram, and why is it important in FT-IR?


Answer: An interferogram is a graphical representation of the interference
pattern produced by the superposition of two or more waves. In the context of
spectroscopy, an interferogram is typically generated by an interferometer,
which splits a beam of light into two or more paths and then recombines them
on a beam splitter to produce an interference pattern.
• It is used When the IR radiation is split into two beams and then
recombined, an interference pattern is produced. The interferogram
represents this interference pattern.
• The interferogram is a time-domain signal, which represents the
interference pattern as a function of time.
• It is used for high precision measurement

Technical Questions
Q: What is a wavenumber, and how is it related to FT-IR?

In FTIR (Fourier Transform InfraRed) spectroscopy, wavenumber (wave
number) is a
crucial concept.
Wavenumber (cm⁻¹) is the reciprocal of wavelength (λ), typically expressed in
centimeters (cm). It’s a measure of the number of waves per unit length.
Wavenumber (ṽ) = 1 / λ
Where λ is the wavelength in centimeters (cm).
Relation to FTIR:
In FTIR spectroscopy, wavenumber is used as the x-axis unit to display the
infrared spectrum. The wavenumber range typically spans from 4000 to 400
cm⁻¹, covering the
mid-infrared region.
Q: How does FT-IR detect functional groups in a molecule?
• Step 1: Infrared Radiation Interaction
• When IR radiation interacts with a molecule, it causes the molecule's
bonds to vibrate. These vibrations occur at specific frequencies, which are
characteristic of the bond type and surrounding molecular environment.
• Step 2: Bond Vibrations
• Different functional groups in a molecule have distinct bond
vibrations, which correspond to specific wavenumber ranges. For example:
• - C-H stretching vibrations occur around 3000-2800 cm−1
• - C=O stretching vibrations occur around 1800-1600 cm−1
• - N-H bending vibrations occur around 1600-1500 cm−1
• Step 3: Absorption of IR Radiation
• When the IR radiation interacts with the molecule, the bonds absorb
radiation at their characteristic frequencies. This absorption causes a
decrease in the transmitted radiation intensity.

• Step 4: Detection and Analysis
• The FT-IR spectrometer detects the absorbed radiation and plots it
against the wavenumber. The resulting spectrum shows peaks corresponding
to the absorbed radiation, which can be assigned to specific functional
groups.

• Step 5: Functional Group Identification
• By analyzing the peaks in the FT-IR spectrum, researchers can identify the
functional groups present in the molecule. This information provides
valuable insights into the molecule's structure, properties, and potential
applications.

Q: What is the difference between absorbance and transmittance


in FT-IR spectra?
In FTIR (Fourier Transform InfraRed) spectroscopy, absorbance and
transmittance are
two related but distinct concepts used to express the interaction between
infrared
radiation and a sample.
Absorbance (A)*
Absorbance is a measure of the amount of infrared radiation absorbed by a
sample.
It’s defined as the logarithmic ratio of the intensity of the incident radiation
(I0) to the
intensity of the transmitted radiation (I):
A = log10 (I0 / I)
Absorbance is typically plotted on the y-axis of an FTIR spectrum, with
higher absorbance values indicating stronger absorption of infrared
radiation.
Transmittance (T)
Transmittance is a measure of the amount of infrared radiation transmitted
through a Sample. It’s defined as the ratio of the intensity of the transmitted
radiation (I) to the intensity of the incident radiation (I0):
T = I / I0

Q: What is a baseline correction, and why is it performed in FT-IR?


• In FT-IR (Fourier Transform InfraRed) spectroscopy, a baseline correction
is a mathematical adjustment made to the spectral data to remove any
unwanted background signals or offsets. This correction is essential to
ensure accurate and reliable spectral interpretation.

Q: Why is baseline correction performed in FT-IR?

• Baseline correction is necessary for several reasons:


• 1. Instrumental background: FT-IR instruments can introduce background
signals due to various instrumental factors, such as detector noise or optical
components.
• 2. Sample background: Samples can also contribute to background signals,
for example, due to scattering or absorption by the sample matrix.
• 3. Atmospheric interference: Water vapor and carbon dioxide in the
atmosphere can absorb IR radiation, leading to unwanted peaks in the
spectrum.
• This correction is important because it ensures that the peaks in the
spectrum accurately reflect the actual absorbance of the sample. Without
baseline correction, you might misinterpret the data, leading to incorrect
conclusions about the sample’s composition. By performing this correction,
you can enhance the clarity of the spectrum and make it easier to identify
the specific functional groups and bonds present in the sample.

• A typical FT-IR (Fourier Transform InfraRed) spectrum represents a plot of


the infrared radiation absorbed or transmitted by a sample as a function of
wavenumber (typically expressed in cm-1). The spectrum provides a
molecular fingerprint of the sample, showing the characteristic absorption
peaks or bands corresponding to specific molecular vibrations.

• The x-axis of the spectrum represents the wavenumber (cm-1), while the y-
axis represents the absorbance or transmittance. The resulting spectrum can
be interpreted to:

• 1. Identify functional groups and molecular structures c=o,N-H,
• 2. Determine the presence of specific chemical bonds
• 3. Analyze the molecular composition of a sample
• 4. Detect impurities or contaminants
• 5. Study chemical reactions and interactions.
Q: What does a typical FT-IR spectrum represent?

A typical FTIR (Fourier Transform InfraRed) spectrum represents the


absorption or Transmission of infrared radiation by a sample as a
function of wavenumber (cm⁻¹).

Components of a Typical FTIR Spectrum:

1. _X-axis_: Wavenumber (cm⁻¹), typically ranging from 4000


to 400 cm⁻¹.
2. _Y-axis_: Absorbance (A) or Transmittance (T), which
represents the intensity of the absorbed or transmitted
infrared radiation.
3. _Spectral Peaks_: Absorption peaks or bands, which
correspond to specific Vibrational modes of the molecules in
the sample.
4. _Spectral Regions_: Different regions of the spectrum, such
as: Hydrogen stretching region (3600-3200 cm⁻¹)
- Carbonyl stretching region (1800-1600 cm⁻¹)
- Fingerprint region (1500-500 cm⁻¹)

_Information Provided by a Typical FTIR Spectrum:_

1. _Molecular structure_: FTIR spectra provide information


about the molecular

Structure of the sample, including the presence of specific functional


groups.

2. _Chemical composition_: FTIR spectra can help identify the


chemical composition

Of a sample, including the presence of specific compounds or


mixtures.
Application Questions

Q: What types of functional groups can be identified using FT-IR?


• FT-IR (Fourier Transform InfraRed) spectroscopy can identify a wide
range of functional groups, including:

• 1. Hydroxyl (-OH): Alcohols, phenols, and carboxylic acids
• 2. Carbonyl (C=O): Aldehydes, ketones, carboxylic acids, and esters
• 3. Amine (-NH2): Primary and secondary amines
• 4. Methyl (CH3) and Methylene (CH2): Alkanes and alkyl groups
• 5. Alkene (C=C) and Alkyne (C≡C): Unsaturated hydrocarbons
• 6. Ester (-COO-): Esters and lactones
• 7. Ether (-O-): Ethers and epoxides
• 8. Nitro (-NO2): Nitro compounds
• 9. Sulfur-containing groups: Thiols, sulfides, and sulfones
• 10. Phosphorus-containing groups: Phosphines, phosphates, and
phosphonates

Q: How can FT-IR be used in identifying unknown compounds?


• 1. Sample preparation: Prepare the unknown compound for FT-IR
analysis, typically by creating a thin film or pellet.
• 2. Data collection: Collect the FT-IR spectrum of the unknown
compound using an FT-IR spectrometer.
• 3. Spectral analysis: Analyze the FT-IR spectrum to identify
characteristic absorption peaks or bands.
• 4. Database searching: Compare the FT-IR spectrum to reference
spectra or databases, such as the Sadtler or Aldrich libraries.
• 5. Matching and identification: Match the FT-IR spectrum to a known
compound, and verify the identification using other analytical techniques,
such as mass spectrometry or nuclear magnetic resonance spectroscopy.

Q: What industries commonly use FT-IR spectroscopy?


• Answer:
• 1. Pharmaceuticals
• 2. Biotechnology
• 3. Chemicals
• 4. Polymers
• 5. Food and Beverage
• 6. Forensic Science
• 7. Environmental Monitoring
• 8. Petrochemicals
• 9. Cosmetics
• 10. Materials Science

Q: How is FT-IR applied in organic chemistry?


• FT-IR spectroscopy is applied in organic chemistry for:

• 1. Functional group identification: Identifying specific functional
groups, such as alcohols, amines, and carbonyls.
• 2. Structural elucidation: Determining the molecular structure of
unknown compounds.
• 3. Reaction monitoring: Monitoring chemical reactions and
identifying reaction products.
• 4. Purity analysis: Verifying the purity of organic compounds.
• 5. Characterization of polymers: Analyzing the molecular structure
and composition of polymers.

Q: What is the importance of FT-IR in environmental analysis?


• 1. Pollutant identification
• 2. Water and air quality monitoring
• 3. Soil analysis
• 4. Waste characterization
• 5. Biodegradation monitoring

Sample Preparation Questions


Q: What are the common methods for sample preparation in FT-
IR?
• The common methods for sample preparation in FTIR are:
• 1. FTIR Solid Sample Preparation
• a. KBr Pellet Method:
• Solid samples are ground into a fine powder and mixed with
potassium bromide (KBr) in a ratio typically around 1:100.
• The mixture is then pressed into a pellet using a hydraulic press. This
pellet is transparent to infrared light.Place the KBr pellet in the sample
holder of the FTIR instrument for analysis.

• b. ATR (Attenuated Total Reflectance) Method:


• The sample is placed in contact with a crystal (often diamond or
germanium) that has a high refractive index.
• - The infrared beam enters the crystal and reflects off the sample
surface, allowing for analysis without extensive sample preparation.

• 2. FTIR Liquid Sample Preparation


• a. Liquid Cell Method:
• - Liquid samples are placed in a liquid cell made of materials like
sodium chloride or calcium fluoride.
• - The thickness of the liquid layer is critical; it should be controlled to
avoid saturation or weak signals.
• b. ATR Method
• Ensure the ATR crystal is clean. Place a drop of the liquid sample
directly onto the ATR crystal.
• Perform the FTIR analysis with the sample in contact with the
crystal.

• 3. FTIR Gas Sample Preparation


• Gaseous samples are analyzed using a gas cell, which is a long path-
length chamber that allows the gas to be contained and measured.
• The design ensures that the gas does not absorb infrared radiation
itself and allows for effective measurement of absorption bands.
• Each of these methods has its advantages and is chosen based on the
specific characteristics of the sample being analyzed.

Q: What is the difference between solid, liquid, and gas sample


preparation for FT-IR?
SOLID LIQUID GAS

Solid samples are Liquid samples are usually Gas samples are typically analy
typically prepared by placed in a liquid cell, which is along path-length chamber th
grinding them into a fine consist of two infrared- measurement of gases.
powder. This can transparent windows (often
increase the surface area made of materials like
for better interaction sodium chloride or calcium
with infrared light. fluoride)
The powdered solid can The thickness of the liquid The gas must be contained in a
be mixed with a non- layer must be controlled to infrared radiation itself, which i
absorbing matrix, like ensure that it is neither too are used for the gas cell.
potassium bromide thick (which can lead to
(KBr), and then pressed saturation) nor too thin
into a pellet. This (which can result in weak
method helps to signals).
minimize scattering and
enhances the clarity of
the spectrum.
Alternatively, solid In some cases some cases, a The concentration of the gas ca
samples can be applied drop of liquid can be placed the absorption bands are detecta
as a thin film on an directly onto a crystal, such saturation.
infrared-transparent as a diamond, for analysis.
substrate.
Q: What is the role of potassium bromide (KBr) in FT-IR sample
preparation?
• Potassium bromide (KBr) is a key component in preparing samples
for Fourier transform infrared (FTIR) spectroscopy because it's optically
transparent in the infrared region and doesn't absorb light in the mid-infrared
range. KBr serves as:
• Carrier
• KBr can be used as a carrier for samples that are difficult to dissolve
in IR-transparent
• Solvents.
• Diluent
• KBr is a diluent that helps achieve clear pellets and consistent diffuse
reflectance results.
• Pellet preparation
• KBr is often mixed with solid samples and pressed into a thin pellet.
This method is commonly used for inorganic compounds.

Q: What is ATR (Attenuated Total Reflectance) in FT-IR, and


how does it simplify sample preparation?
Answer: ATR stands for Attenuated Total Reflectance, and it is a technique
used in FTIR (Fourier Transform Infrared Spectroscopy) that simplifies
sample preparation significantly. Here's how it works;
• 1. Principle of ATR: In ATR, the infrared beam is directed onto an
internal
• reflection element (IRE), typically made of materials like zinc
selenide or diamond. The beam penetrates the sample in contact with the
IRE at a shallow depth, typically only a few micrometers. This allows for
the analysis of samples without needing to prepare them as thin films or
pellets.
• 2. Simplified Sample Preparation: One of the main advantages of
ATR is that it eliminates the need for extensive sample preparation. You can
analyze solid, liquid, and even paste-like samples directly without the need
to mix them with KBr or other matrices, which is required in traditional
FTIR methods.

• 3. Versatility: ATR can handle a wide variety of samples, including
powders, gels, and liquids, making it a versatile choice for many
applications. This adaptability reduces the time and effort needed to prepare
samples for analysis.
• 4. Reduced Contamination Risk: Since samples can be analyzed
directly on the IRE, there is a lower risk of contamination compared to
traditional methods where samples might be handled multiple times.
• 5. Quick Analysis: ATR allows for rapid data collection, as there's
no need to press pellets or create films, making the overall process more
efficient.
Q: What precautions are necessary when preparing samples for
FT-IR?
Answer: When preparing samples for FTIR analysis, it's important to take
several precautions to ensure accurate results and avoid contamination.
Following are the precaution that can follow to enhance the reliability and
accuracy of FTIR.

• 1. Cleanliness: Ensure that all glassware, tools, and surfaces used in


the preparation are clean and free from contaminants. Residues from
previous samples can interfere with the analysis.
• 2. Sample Handling: Use gloves when handling samples to prevent
contamination from oils and residues on your skin. Avoid touching the
sample or KBr pellets directly.
• 3. Moisture Control: KBr is hygroscopic, meaning it can absorb
moisture from the air. Store KBr in a desiccator and minimize exposure to
humidity to prevent changes in its properties.
• 4. Sample Size: Use the appropriate amount of sample when
preparing pellets or films. Too much sample can lead to saturation of the
spectrum, while too little may not provide a detectable signal.
• 5. Pressing Technique: When making KBr pellets, apply even
pressure to avoid cracks or inconsistencies in the pellet. A well-formed
pellet is crucial for accurate results.

Advanced Questions:
Q: What is the advantage of using Fourier Transform in FT-IR?
The advantage of using Fourier transform in FTIR spectroscopy are:
• HIGHER SENSITIVITY: The Fourier transform enhances the
sensitivity of the measurements, allowing for the detection of weaker signals
and smaller amount of sample material.
• FASTER SCANNING: It can collect data quickly because it
captures all wavelengths simultaneously rather than one at a time.
• IMPROVE SPECTRAL RESOLUTION: The Fourier transform
enables the calculation of high spectral resolution, allowing for better
separation of closely spaced spectral peaks.
• SIGNAL-TO-NOISE RATIO: The use of Fourier transform
technique improve the signal-to-noise ratio, resulting in clearer and more
reliable spectra.
• INCREASED ACCURACY: Through Fourier transform we get
more precise and reliable spectral data.
Q: How does FT-IR compare with dispersive IR spectroscopy?

FT-IR SPECTROSCOPY DISPERSIVE IR


SPECTROSCOPY
1 In order to measure an IR In order to measure an IR
spectrum, FTIR takes only a spectrum, the dispersion
few seconds. spectrometer takes several
minutes.
2 It gives higher sensitivity and It gives lesser sensitivity.
precision.
3 In FT-IR only the mirror There are many moving parts,
moves during the experiment. resulting in mechanical slippage.
4 In FT-IR spectroscopy we use In dispersive IR spectroscopy we
Michelson interferometer. use monochromator.
5 Use of laser provides high Calibration against refrence
frequency accuracy. spectra is required to measure
frequency.
6 Faster than dispersive IR Slower than FT-IR spectroscopy.
spectroscopy.

Q: What are the limitations of FT-IR spectroscopy?


LIMITATIONS OF FTIR:
• It cannot be used to detect all the vibration modes in a molecule.
• It is not possible to know molecular weight of substance
• It is not possible to know whether it is pure compound or a mixture of
compound.
• Interferogram are difficult to interpret without first performing a
Fourier transform to produce a spectrum.
• Accuracy of FT-IR remains true if there is no change in atmospheric
conditions throughout the experiment.

Q: What factors affect the accuracy of FT-IR spectra?


FACTORS AFFECT ACCURACY OF FT-IR SPECTRA:
The accuracy of FT-IR spectra is affected by several factors, including:
• INSTRUMENT QUALITY: The quality and calibration of the FT-
IR instrument is a significant factor in the accuracy of the analysis. Any drift
in the instrument’s parameters can affect the accuracy of the spectral data.
• SAMPLE PREPARATION: The way a sample is prepared can
significantly influence the results. Inhomogeneities, contaminants, or
improper thickness can lead to inaccurate spectra.
• RESOLUTION: The resolution of the FT-IR spectrometer must
must be appropriately set for the analysis being conducted. Too low a
resolution may lead to loss of detail, while too high a resolution can increase
noise.
• ENVIRONMENTAL CONDITION: Factors such as temperature,
humidity, and atmospheric pressure can impact the FT-IR measurements.
For Example, water vapor in the environment can interfere with the infrared
signals.
• DETECTOR SENSITIVITY: The sensitivity and response of the
detector used in the FTIR system can also affect the accuracy. A less
sensitive detector may not pickup weak signals effectively.

Q: How can FT-IR be used in quantitative analysis?


• FT-IR can be used in quantitative analysis through the following
methods:
• 1. Calibration Curves: A series of standard solutions with known
concentrations of the analyte can be prepared. The FT-IR spectra of these
standards are collected, and the absorbance (or transmittance) at specific
wavelengths is plotted against concentration to create a calibration curve.
The concentration of unknown samples can then be determined by
measuring their absorbance and comparing it to the calibration curve.
• 2. Beer-Lambert Law: The quantitative analysis can be based on the
Beer-Lambert law, which states that absorbance is directly proportional to
concentration. The equation A = εlc is used, where A is absorbance, ɛ is the
molar absorptivity, I is the path length, and c is the concentration. By
knowing ε and I, the concentration of an unknown sample can be calculated
from its measured absorbance.
• 3. Peak Area or Height Measurement: In some cases, the area
under the absorption peak or the height of the peak can be used to quantify
the amount of analyte present. This method is particularly useful for
complex mixtures where multiple components are present.
• 4. Multivariate Calibration: For complex samples, multivariate
techniques such as Principal Component Analysis (PCA) or Partial Least
Squares (PLS) can be employed. These methods analyze the spectral data
from multiple wavelengths simultaneously to improve the accuracy of
concentration predictions.
• 5. Internal Standards: The use of an internal standard, a compound
that is added in a known amount to the sample, can help improve the
accuracy and precision of the quantitative analysis by compensating for
variations in sample preparation or instrument response.
• By employing these methods, FT-IR can effectively be used for
quantitative analysis in various fields, including pharmaceuticals,
environmental monitoring and food quality control.
Q: How does the Fourier Transform convert an interferogram into
an IR spectrum?
• The Fourier transform is a mathematical technique that converts a
signal from its original domain (often time or space) into the frequency
domain. The method by which Fourier transform convert an interferogram
into an infrared (IR) spectrum is;
• 1. Interferogram: When you perform an IR spectroscopy
experiment, the sample is exposed to infrared light. The light is split into
two beams, and after reflecting off the sample and a mirror, the beams are
recombined. This creates an interferogram, which is essentially a time-
domain signal representing the intensity of light as a function of the path
difference between the two beams.
• 2. Time Domain to Frequency Domain: The interferogram contains
information about the different frequencies (or wavelengths) of light
absorbed by the sample. To extract this information, apply the Fourier
transform to the interferogram. The Fourier transform decomposes the time-
domain signal into its constituent frequencies.

• 3. Spectrum Generation: The result of the Fourier transform is a
spectrum that displays the intensity of light absorbed by the sample as a
function of frequency (or wavelength). Peaks in this spectrum correspond to
specific molecular vibrations and transitions in the sample, allowing for the
identification of different chemical species.
•  The Fourier transform takes the raw interferogram data, which is a
time-domain representation, and converts it into a frequency-domain
representation, resulting in an IR spectrum that reveals the chemical
composition of the sample.

Q: What are the advantages of using interferometry in FT-IR compared to


dispersive spectroscopy?

The advantages of using interferometry in FT-IR spectroscopy over dispersive


spectroscopy are:
• Speed: FT-IR can acquire the entire spectrum simultaneously rather than
scanning through each wavelength one at a time as in dispersive
spectroscopy. This leads to much faster data collection.
• Sensitivity: FT-IR is generally more sensitive than dispersive methods. It
can detect lower concentrations of analytes because it collects more data in a
single measurement.
• Resolution: FT-IR can achieve higher spectral resolution due to the use of a
Michelson interferometer, which allows for precise control over the path
length difference between the two beams of light.
• Signal-to-Noise Ratio: The technique benefits from a higher signal-to-noise
ratio due to the co-addition of multiple scans, which averages out noise and
enhances the quality of the spectrum.
• No Moving Parts: the interferometer is designed with fewer moving parts
compared to dispersive system, leading to potentially lower maintenance
and greater reliability.

Fill in the blanks using the given words.


1. The main function of the beam splitter interferometer in an FT-IR
spectrometer is to split the infrared beam into two parts.
2. FT-IR spectrometers typically use a Michelson interferometer for creating
interference patterns.
3. The moving mirror in an FT-IR interferometer is responsible for creating an
optical path difference.
4. The detector in FT-IR detects the intensity of infrared radiation transmitted
or reflected by the sample.
5. FT-IR uses an broadband source to emit infrared light.
6. The mirrors is used to focus infrared light onto the detector in FT-IR
systems.
7. The sample compartment in FT-IR is where the sample is placed to interact
with the infrared radiation
8. In FT-IR, the beam splitter is used to recombine the split beams after they
pass through the sample.
9. The optics ensures that infrared radiation is transmitted through or reflected
from the sample during FT-IR analysis.
10. The Fourier transform is responsible for generating a spectrum from the
interferogram.
11. In FT-IR, the laser provides a reference signal used for calibrating the
instrument.
12. The beam splitter in FT-IR is typically made from KBr or other
infraredtransmitting materials.
13. The fixed mirror in FT-IR remains fixed while the other mirror moves.
14. The filter is often used to reduce the amount of infrared radiation reaching
the sample.
15. The Fourier Transform is applied to the interferrogram to convert the time-
domain data into an IR spectrum.
16. The beam splitter in FT-IR directs light to the sample and then reflects it
back to the detector.
17. The infrared light that interacts with the sample is often transmitted through
a window before entering the sample compartment.
18. FT-IR instruments typically have a pyroelectric or thermocouple detector
for detecting infrared light.
19. The gas cell compartment is used for analyzing gases in FT-IR
spectroscopy.
20. FT-IR spectrometers commonly use moving mirrors for their adjustable
positioning in the interferometer.
Laser - Fixed - Beam splitter - KBr (potassium bromide) - Infrared
radiation – Interferogram – Filter – Detector -Infrared light -Thermocouple
or Pyroelectric –Lens -Optical - Gas cell - Fourier transform – Adjustable –
Michelson –Window -Infrared source-Sample compartment - Moving mirror

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