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    FT-IR Analysis of Materials

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    ricky
    This document provides an overview of Fourier transform infrared (FT-IR) spectroscopy. It discusses the importance of IR spectroscopy for identifying organic and inorganic compounds and functional groups. The working principle is described as molecules absorbing IR radiation based on their natural vibrational frequencies. The instrumentation of modern FT-IR spectrometers is explained, including their use of interferometers and how an interferogram is obtained and transformed to a spectrum. Common sampling methods like transmission, ATR, and grazing angle are outlined. The document concludes with an example case study of using FT-IR to analyze surface functionalization of polyethylene.

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    © All Rights Reserved
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    FT-IR Analysis of Materials

    Uploaded by

    ricky
    128 views50 pages
    This document provides an overview of Fourier transform infrared (FT-IR) spectroscopy. It discusses the importance of IR spectroscopy for identifying organic and inorganic compounds and functional groups. The working principle is described as molecules absorbing IR radiation based on their natural vibrational frequencies. The instrumentation of modern FT-IR spectrometers is explained, including their use of interferometers and how an interferogram is obtained and transformed to a spectrum. Common sampling methods like transmission, ATR, and grazing angle are outlined. The document concludes with an example case study of using FT-IR to analyze surface functionalization of polyethylene.

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    This document provides an overview of Fourier transform infrared (FT-IR) spectroscopy. It discusses the importance of IR spectroscopy for identifying organic and inorganic compounds and functional groups. The working principle is described as molecules absorbing IR radiation based on their natural vibrational frequencies. The instrumentation of modern FT-IR spectrometers is explained, including their use of interferometers and how an interferogram is obtained and transformed to a spectrum. Common sampling methods like transmission, ATR, and grazing angle are outlined. The document concludes with an example case study of using FT-IR to analyze surface functionalization of polyethylene.

    Copyright:

    © All Rights Reserved
    Download as PPTX, PDF, TXT or read online from Scribd
    Download as pptx, pdf, or txt
    128 views50 pages

    FT-IR Analysis of Materials

    Uploaded by

    ricky
    This document provides an overview of Fourier transform infrared (FT-IR) spectroscopy. It discusses the importance of IR spectroscopy for identifying organic and inorganic compounds and functional groups. The working principle is described as molecules absorbing IR radiation based on their natural vibrational frequencies. The instrumentation of modern FT-IR spectrometers is explained, including their use of interferometers and how an interferogram is obtained and transformed to a spectrum. Common sampling methods like transmission, ATR, and grazing angle are outlined. The document concludes with an example case study of using FT-IR to analyze surface functionalization of polyethylene.

    Copyright:

    © All Rights Reserved
    Download as PPTX, PDF, TXT or read online from Scribd
    Download as pptx, pdf, or txt
    of 50

    FT-IR - Fourier Transform InfraRed

    FT-IR Spectroscopy & Analysis of Materials


    Mrs. Purvi Kikani
    Dave

    10/5/16

    Presentation Over View


    Importance of IR Spectroscopy
    Working Principle of IR Spectroscopy
    Instrumentation
    Sampling Methods & Sample Criteria
    How to Read Infra-Red Spectra ?
    Case

    Study

    Surface

    Activation

    of

    polyethylene by plasma
    10/5/16

    Importance of IR
    Spectroscopy
    IR Spectroscopy is used for qualitative
    identification of organic and inorganic
    compounds.
    IR Spectroscopy is used for checking
    presence of functional groups in organic
    compounds.
    Wavenumber with
    commonly used
    Wavenumber
    10/5/16

    units

    number

    of

    of

    cm-1

    is

    waves

    of3

    Working Principle of IR
    Spectroscopy
    Molecules are made up of atoms
    linked by chemical bonds.
    A diatomic molecule is considered as
    a two spherical masses (m1 & m2)
    connected with a spring with a given
    force constant f.

    ~ 1 f
    2c
    10/5/16

    Working Principle of IR
    Spectroscopy
    This characteristic vibrations are
    called Natural frequency of vibration
    Applied Freq. = Natural Freq. of
    Vibration
    Absorption of IR radiation takes place
    and a peak is observed.
    10/5/16

    IR Absorption in 2-Hexanone

    10/5/16

    Basics of IR Spectroscopy
    IR Absorption & Bond Vibration in 2 - Hexanone

    The vibrations of a 2-hexanone molecule are


    not, of course, limited to the simple stretching
    of the carbonyl bond. The various carboncarbon bonds also stretch and bend, as do the
    10/5/16
    7
    carbon-hydrogen
    bonds.

    IR Spectra of 2 - Hexanone

    Functional Group Region


    10/5/16

    Instrumentation / Hardware
    A source - which provides the electromagnetic
    energy required for the analysis
    A signal sorter (a dispersion or interference
    device for resolving the frequencies from each
    other).
    A sample compartment
    A signal detector
    A computer
    analysis).
    10/5/16

    (for

    data

    acquisition

    and
    9

    Instrumentation / Hardware
    Older Generation Instrument- A Dispersive IR
    Spectrometer

    Takes 10 20
    minutes to scan
    entire range

    Scanning instrument uses a frequency separation


    device (grating) to resolve the IR radiation into
    individual frequencies.
    An exit slit isolates
    a specific frequency for
    passage to the sample
    10/5/16
    10

    Modern IR Spectrometer Optical


    Design
    Light
    source

    Movable mirror

    He-Ne gas laser

    Beam splitter

    Interferogra
    m
    Sample chamber

    Fixed mirror

    Detector

    Interferometer
    10/5/16

    11

    Relative Intensity

    Fourier Transform of an Interferogram


    yields a Spectrum

    Optical Path Difference

    10/5/16

    Wavenumbers cm-1

    12

    Measuring a typical IR Spectra

    % T = 100 x
    I/I0

    10/5/16

    13

    Sampling Methods
    Available with our instrument

    Transmission
    ATR
    Grazing Angle

    10/5/16

    14

    Transmission Method
    Thin Films
    Solids (pallet
    Technique)

    10/5/16

    15

    Sample criteria
    for Transmission Method
    For Analyzing Thin Films:
    Film should be in the free standing
    condition and thickness should be 50m
    For Analyzing Solids by Pallet Technique:
    In this technique, a small amount of finely
    ground solid sample is mixed with 100
    times its weight of potassium bromide and
    compressed into a thin transparent pellet
    using a hydraulic press.
    10/5/16

    16

    ATR Sampling Method

    The infrared radiation interacts with the sample


    through series of standing waves called
    evanescent waves.
    An evanescent wave is produced each time the
    infrared beam is reflected from the inside surface
    of the crystal
    10/5/16
    The evanescent waves penetrate the sample at17

    How ATR method works ?


    IR beam is directed into a crystal of relatively
    higher refractive index (mostly 2).
    IR beam reflects from the internal surface of the
    crystal and creates an evanescent wave which
    projects orthogonally in to the sample in intimate
    contact with the ATR crystal
    Some of the energy of evanescent wave is
    absorbed by the sample and reflected radiation
    is returned to the detector.
    10/5/16

    18

    Sample criteria for ATR


    Method

    We can analyze following type of samples


    Soft polymers
    Rubbers
    Soft powders
    Pastes
    Gels
    Surface coatings
    Aqueous liquids

    10/5/16

    19

    Sample criteria for ATR


    Method

    We can Not analyze following type of


    samples
    Hard polymers
    Fibers
    Hard powders
    Films on Metals
    Brittle / Grindable solids
    Acidic liquids
    Caustic liquids
    10/5/16

    20

    SAGA Sampling Method


    Specular Apertured Grazing Angle
    Specular reflection is defined as light
    reflecting from a smooth surface (such as
    mirror) at a definite angle

    Specular reflectance is a non-destructive method


    for surface measurements using a mirror like
    reflection from shiny sample surface.
    This method is used for analysis of thin films
    deposited on reflective surfaces with thickness
    1m 10 A
    10/5/16

    21

    How to Read / Interpret an IR


    Spectra ??

    2.
    What
    Functional
    Groups are Present in
    the
    material under
    test ?

    Functional Group Region


    10/5/16

    1.Which is
    the
    material
    under
    test
    ?
    (identifying
    unknown
    material)

    Fingerprint Region
    22

    What do we mean by Functional


    Groups
    ?? of atoms with
    A functional group
    is a group
    specific physical

    & chemical properties. It is

    reactive part of the molecule.


    Most organic compounds have C C and C H
    bonds.
    However many organic compound possess other
    structural features such as;

    Contains
    otherfor
    These specific
    structuralheteroatoms
    features are(atoms
    responsible
    chemical than
    reactivity
    C / H) of a molecule ; hence these
    structures are known as functional groups
    Contains bonds
    10/5/16
    23

    How functional groups make the molecule


    reactive ?

    Ethane contains only C- C and C-H bonds; hence it has


    no heteroatoms / bonds and so no reactive sites Non
    Reactive Nature
    Ethanol contains OH molecule attached. It contains
    heteroatoms which has two lone pairs of electrons which
    make it Reactive in nature.
    10/5/16

    24

    How to identify unknown


    The region to the right-hand
    side of the
    material
    ??diagram (from

    about

    1500 to 500 cm-1) usually contains a very complicated series of


    absorptions. These are mainly due to all manner of stretching
    & bending vibrations within the molecule. This is called the
    fingerprint
    region.
    It
    is much more
    difficult to pick out individual bonds in this
    region than it is in the "cleaner" region at higher wavenumbers.
    The importance of the fingerprint region is that each different
    compound produces a different pattern of peaks in this
    part of the spectrum.

    Fingerprint Region

    How fingerprint region is important in


    identifying unknowns ?

    How to know what kind of functional


    groups are present in material under
    test ??

    onal group region is divided in to 5 zones for better understa

    Zone 1

    3200 3700
    cm -1

    10/5/16

    Alcohols ( -- OH group)
    Alkynes ( C H)
    N-H Stretching (N H)

    Functional Group Region

    27

    How to know what kind of functional


    groups are present in material under
    test ??
    Zone 2

    Aldehydes ( -- CHO)
    Carboxylic acids (-- COOH)

    2700 3200
    cm -1

    10/5/16

    Functional Group Region

    28

    How to know what kind of functional


    groups are present in material under
    test ??
    Zone 3

    Alkynes ( C C)
    Nitriles(C N)

    2000 2300
    cm -1

    10/5/16

    Functional Group Region

    29

    How to know what kind of functional


    groups are present in material under
    test ??
    Carbonyls (-C=O)

    Zone 4

    1650 1800
    cm -1

    Functional Group Region

    How to know what kind of functional


    groups are present in material under
    test ??
    Alkenes
    ( C=C)

    Zone 5

    1680 1620
    cm -1

    Functional Group Region

    Case Study
    Surface Functionalization of Polyethylene

    10/5/16

    32

    Case Study
    Surface Functionalization of Polyethylene
    1720 cm
    --C=O

    10/5/16

    -1

    1640 cm

    -1

    C=C

    33

    Case Study
    Surface Functionalization of Polyethylene

    10/5/16

    34

    Thank you

    10/5/16

    35

    Resolution

    10/5/16

    In order to resolve two


    peaks in a spectrum
    three data points are
    needed. One on each
    peak and one point in
    between.
    Data point spacing is
    controlled
    by
    resolution
    parameter
    and
    is

    the
    At resolution 4 cm-1,
    resolution.
    OPD is 0.25 cm and
    mirror movement is
    0.125 cm
    36

    Why there is He-Ne Laser in FT-IR ?


    Interferogram is not recoded continuously, but sampled at discrete
    intervals to give different data points. The closer the spacing between
    data points, the greater the wavenumber range of the spectrum.
    Monochromatic visible He-Ne laser beam is passed along with the
    polychromatic IR light to provide a single wavelength interferogram
    that oscillates much more quickly than anything in the IR (shorter
    wavelength).

    The laser is used as an


    internal clock to trigger
    data points acquisition
    events.
    IR data points might be
    taken at every zero point
    of
    the
    laser
    interferogram.
    10/5/16

    37

    DIPOLE MOMENT ()
    =Qxr
    Q = charge and r = distance between charges
    - Asymmetrical distribution of electrons in a bond renders the
    bond polar
    - A result of electronegativity difference
    - changes upon vibration due to changes in r
    - Change in with time is necessary for a molecule to absorb
    IR radiation

    DIPOLE MOMENT ()
    - The repetitive changes in makes it possible for polar molecules
    to absorb IR radiation
    - Symmetrical molecules do not absorb IR radiation since they
    do not have dipole moment (O2, F2, H2, Cl2)
    - Diatomic molecules with dipole moment are IR-active
    (HCl, HF, CO, HI)
    - Molecules with more than two atoms may or may not be
    IR active depending on whether they have permanent
    net dipole moment

    10/5/16

    40

    Force constant for chemical


    bonds

    10/5/16

    41

    Energy Distribution Curves for IR


    Source

    10/5/16

    42

    Out put of an interferometer =


    Interferogram
    An interferogram has every
    infrared
    frequency
    (or
    wavelength) encoded in it

    An
    interferogram
    containing all IR
    frequencies now
    enters
    the
    sample
    compartment
    10/5/16

    43

    Absorbance / Transmittance
    A Beer Lambert Law

    absorptivity coefficient) x b (path length) x c (concent

    10/5/16

    44

    Factors Affecting ATR


    Spectra
    Refractive indices of the ATR crystal and
    sample
    Depth of penetration
    Effective path length
    Number of reflections
    Quality of sample contact with ATR crystal

    10/5/16

    45

    Some Common Functional Groups

    10/5/16

    46

    Modes of vibrations
    Region

    antisymmetric
    R
    R
    R

    symmetric

    H
    H
    H

    R
    H
    scissoring

    R
    H
    rocking

    Origin of the absorption

    Overtones and combination


    bands of fundamental
    molecular vibrations

    MIR

    fundamental molecular
    vibrations

    FIR

    molecular rotations

    stretching

    in-plane
    bending

    H
    H

    NIR

    bending

    Molecule

    Degrees of
    freedom

    Non linear
    Linear

    3N -6
    3N- 5

    The Absorption Techniques of MIR and NIR


    Spectroscopy
    The Harmonic Oscillator

    The simplest classical model employed to have a didactic


    insight on the interaction of radiation and matter in the NIR
    spectral region depicts a diatomic molecule as two spherical
    masses (m1 and m2) connected with a spring with a given
    force constant (k). Hooks law states that the energy (E) of
    this system is given by:

    V
    -A
    0
    +A

    E = (h/2)(k/)

    where is the reduced mass.

    The molecular vibration can be described by a simplified


    model supposing a harmonic oscillator for which the
    potential energy (V), as a function of the displacement of
    the atoms (x), is given by:
    -A

    0
    Displaceme
    nt

    +A

    V = kx2

    The potential energy curve of such an oscillator is parabolic


    in shape and symmetrical about the equilibrium bond length.

    Harmonic Oscillator prepared by Carlos Ortega

    The Absorption Techniques of MIR and NIR


    Spectroscopy
    For the harmonic oscillator the energy levels are equidistant and transitions are only allowed between
    neighboring energy levels with:

    n = 1

    According to the Boltzmann distribution, most molecules at room temperature populate the ground level n
    = 0, and consequently the allowed, so-called fundamental, transitions between n = 0 and n = 1 dominate
    the vibrational absorption spectrum.

    For the harmonic oscillator n = 1 and Ep = hv, which matches the predicted equal energy difference
    between one state and the other of immediately higher energy. The figure at right shows the effect of
    photon absorption on the energy and amplitude of vibration.

    Fundamentals and Overtones

    In the case of the anharmonic


    oscillator,
    the
    vibrational
    transitions no longer only obey
    the selection rule n = 1. This
    type of vibrational transition is
    called fundamental vibration.
    Vibrational transitions with n =
    2, 3, ... are also possible, and
    are termed overtones. Called
    first, second, and so on,
    overtones.

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