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    Experiment 2: Determination of A Mixture of Xylene Isomers Using Infrared (Ir) Spectrometer

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    Nur Atiqah Mohd Redzuan
    The document describes an experiment to determine the mixture of xylene isomers (ortho-, meta-, and para-) in a sample using infrared spectrometry. Standard solutions containing varying concentrations of the three isomers were prepared and their infrared spectra were recorded and analyzed using a baseline technique. The procedure and results of analyzing standard solutions, pure isomers, and an unknown sample are presented.

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    Experiment 2: Determination of A Mixture of Xylene Isomers Using Infrared (Ir) Spectrometer

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    Nur Atiqah Mohd Redzuan
    874 views8 pages
    The document describes an experiment to determine the mixture of xylene isomers (ortho-, meta-, and para-) in a sample using infrared spectrometry. Standard solutions containing varying concentrations of the three isomers were prepared and their infrared spectra were recorded and analyzed using a baseline technique. The procedure and results of analyzing standard solutions, pure isomers, and an unknown sample are presented.

    Original Description:

    EXPERIMENT 2 SKA3023

    Original Title

    Experiment 2

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    The document describes an experiment to determine the mixture of xylene isomers (ortho-, meta-, and para-) in a sample using infrared spectrometry. Standard solutions containing varying concentrations of the three isomers were prepared and their infrared spectra were recorded and analyzed using a baseline technique. The procedure and results of analyzing standard solutions, pure isomers, and an unknown sample are presented.

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    874 views8 pages

    Experiment 2: Determination of A Mixture of Xylene Isomers Using Infrared (Ir) Spectrometer

    Uploaded by

    Nur Atiqah Mohd Redzuan
    The document describes an experiment to determine the mixture of xylene isomers (ortho-, meta-, and para-) in a sample using infrared spectrometry. Standard solutions containing varying concentrations of the three isomers were prepared and their infrared spectra were recorded and analyzed using a baseline technique. The procedure and results of analyzing standard solutions, pure isomers, and an unknown sample are presented.

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    of 8

    EXPERIMENT 2: DETERMINATION OF A MIXTURE OF XYLENE ISOMERS

    USING INFRARED (IR) SPECTROMETER

    Objectives:

    Upon completion of this experiment, students should be able to:

    1. Prepare samples for IR analysis


    2. Measure Po/p using baseline
    3. Perform IR analysis on aqueous solutions

    Introduction:

    Meta- and para-xylene are determined in mixture using ortho-xylene as an internal standard
    to compensate for variation in cell length between runs. The infrared spectrum of the
    unknown mixture is recorded and the relative height of peaks of the two compounds are
    compared with those of standard mixture, using the baseline technique. The chemical
    structures of ortho-, meta- and para-xylene are shown in figure below:

    Chemicals and Apparatus:

    Chemicals:

    Ortho-xylene

    Meta-xylene

    Para-xylene

    Cyclohexane
    Apparatus:

    Beaker (100 mL)

    Micropipette

    Procedure:

    Part A: Preparation of solutions

    1. Provided. Ortho-, meta- and para-xylene


    2. To prepare. A series of standard solutions in 10 mL volumetric flask was prepared,
    following the volume of isomers as depicted in table below:

    Volume of isomer (mL)


    Xylene isomer
    I II III IV
    Ortho- 0.2 0.2 0.2 0.2
    Meta- 0.1 0.2 0.3 0.5
    Para- 0.5 0.3 0.2 0.1

    3. To each of the volumetric flask, cyclohexane was added to the mark

    Part B: UV-Visible analysis

    1. Consult your lab assistant, prior to operate of your instrument


    2. The infrared cell was handled carefully, avoiding contact with water and the fingers
    3. Spectra on each of the following solution from 2000 to 650 cm-1 was ran:
    i. Solution of 50% (vol/vol) o-xylene in cyclohexane
    ii. Solution of 50% (vol/vol) m-xylene in cyclohexane
    iii. Solution of 50% (vol/vol) p-xylene in cyclohexane
    iv. Standard solutions I-IV
    v. Pure cyclohexane solvent
    vi. Unknown solution
    4. From the spectra of the pure substances, a peak of each isomer to measure was chosen
    5. Using the baseline method, Po/P was measured for the peak for each compound
    6. An unknown mixture of isomers was obtained from our lab assistant. The spectrum
    was ran on this mixture and using the baseline method, Po/P for three compound was
    measured

    Results:

    Part A: Absorbance peaks of infrared for xylene isomers

    Xylene isomer Peak (cm-1)


    o-xylene 696.78
    m-xylene 767.57
    p-xylene 794.01

    Part B: Absorbance (log Po/P) for xylene isomers

    o-xylene isomers

    Solution % o-xylene Po P log Po/P (x 10-3)


    I 2 99.76 97.75 8.84
    II 2 99.75 97.75 8.80
    III 2 99.81 97.63 9.59
    IV 2 98.13 96.25 8.40
    Unknown 98.13 96.13 8.94

    m-xylene

    Solution % m-xylene Po P log Po/P (x 10-3)


    I 1 99.76 99.10 2.88
    II 2 99.75 98.31 6.32
    III 3 99.81 98.00 7.95
    IV 5 99.75 96.20 15.74
    Unknown 98.19 90.25 36.62

    p-xylene

    Solution % p-xylene Po P log Po/P (x 10-3)


    I 5 100.00 96.90 13.68
    II 3 99.88 98.13 9.68
    III 2 100.0 98.69 5.73
    IV 1 99.50 93.19 28.43
    Unknown 97.94 96.25 7.56

    Solution of 50% (vol/vol) o-xylene in cyclohexane

    % o-xylene Po P log Po/P


    50 97.63 89.75 0.0365

    Solution of 50% (vol/vol) m-xylene in cyclohexane

    % m-xylene Po P log Po/P


    50 99.19 84.25 0.0709

    Solution of 50% (vol/vol) p-xylene in cyclohexane

    % p-xylene Po P log Po/P


    50 98.63 82.00 0.0802
    Discussion:

    In this experiment, we are able to determine the mixture of xylene isomers that consisit
    of ortho-, meta- and para-xylene using infrared spectrometry. There are two types of spectra
    that we obtained from this experiment. The first type of spectra is comparing the standard I-
    IV with pure ortho-, meta- and para-xylene. We compared both spectra based on the nearest
    value in each pure xylene compound. The second type of spectra is comparing the pure
    xylene and cyclohexane with the solution of cyclohexane.

    Based on the two types of spectra, we can see that there are other substances other than
    ortho-, meta- and para-xylene itself. The absorption peaks within IR region are ususally
    sharper compared with absorption pekas from ultraviolet and visible region. From both
    spectra, we obtained the value of Po, P and log Po/P using the baseline method.
    Conclusion:

    The samples for IR analysis was prepared. Po/P was measured using baseline method.
    IR analysis was performed on aqueous solution.

    References:

    Chemistry Libretext. (2019). Infrared: Theory. Retrieved from


    https://chem.libretexts.org/Bookshelves/Physical_and_Theoretical_Chemistry_Textbook_
    Maps/Supplemental_Modules_(Physical_and_Theoretical_Chemistry)/Spectroscopy/Vibr
    ational_Spectroscopy/Infrared_Spectroscopy/Infrared%3A_Theory

    Pharmatutor. (2008). Define and differentiate between auxochromes and chromophores.


    Exemplify and explain how auxochrome shifts. Retrieved from
    https://www.pharmatutor.org/pharma-analysis/define-and-differentiate-between-
    auxochromes-and-chromophores-exemplify-and-explain-how-auxochrome-hifts

    Thermo Scientific. (2008). Advantages of a Fourier Transform Infrared Spectrometer.


    Retrieved from https://assets.thermofisher.com/TFS-Assets/LSG/Application-
    Notes/TN50674-E-0215M-FT-IR-Advantages.pdf
    Questions:

    1. What is the criterion for absorption to occur in the infrared region?


    - A criterion for IR absorption is a net change in dipole moment in a molecule
    as it vibrates or rotates.

    2. What types of molecular vibration are associated with infrared absorption?


    - Vibration fall into the basic categories which are stretching and bending. A
    stretching vibration involves a continuous change in the interatomic distance
    along the axis of the bond between two atoms. Bending vibrations are
    characterized by a change in the angle between two bonds and there are four
    types which are scissoring, rocking, wagging and twisting.

    3. Define the following terms:


    a. Chromophore: a group of atoms and electrons forming part of an organic
    molecule that causes it to be colored
    b. Auxochrome: It is a group which itself does not act as a chromophore but
    when attached to a chromophore, it shifts the adsorption towards longer
    wavelength along with an increase in the intensity of absorption
    c. Bathchromic shift: a shift of a band to lower energy or longer wavelength
    (often called a red shift)
    d. Hypsochromic shift: a shift of a band to higher energy or shorter
    wavelength (often called a blue shift)
    e. Hyperchromism: an increase in the molar absorptivity
    f. Hypochromism: an decrease in the molar absorptivity
    4. Sulfur dioxide is a non-linear molecule. How many vibrational model will this
    compound have? How many absorption peaks would sulfur dioxide be
    expected to have?
    - the number of modes of vibrations for a non-linear molecule is 3N-6. The
    number of modes for sulfur dioxide is:
    3 N−6=3 ( 3 )−6=3
    - there are three absorption peaks will sulfur dioxide be expected to have

    5. What are the advantages of Fourier transform infrared (FTIR) spectrometer


    compared to a dispersive instrument?
    - Multiplex advantage: many scans can be completed and averaged on an FTIR
    in a shorter time than one scan on most dispersive instruments
    - Throughput advantage: more energy reaches the samples and hence the
    detector in an FTIR spectrometer than in a dispersive spectrometer
    - Precision advantage: an FTIR spectrometer uses a laser to control the velocity
    of the moving mirror and to time the collection of data points throughout the
    mirror stake

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