DEPARTMENT OF CHEMISTRY

FACULTY OF SCIENCE OF MATHEMATICS

LAB REPORT
ANALYTICAL CHEMISTRY 2
SKA 3023

EXPERIMENT 2

DETERMINATION OF A MIXTURE OF XYLENE ISOMERS USING

INFRARED (IR) SPECTROMETER)
1

NAME OF GROUP MEMBERS: MATRIC NO:

AIN SUFIZA BINTI NORMAN ZAIRI D20171078202

SITI AISYAH BINTI SHA’ARI D20171078204

DAY/TIME 19 NOVEMBER 2019 ( 8- 11 AM)

LABORATORY B3-3-MK 13

LECTURER ‘S NAME DR. MAZLINA BINTI MUSA

EXPERIMENT 2

DETERMINATION OF A MIXTURE OF XYLENE ISOMERS USING INFRARED (IR)

SPECTROMETER

OBJECTIVES:

1. Prepare samples for IR analysis.

2. Measure Po/P using baseline method.
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 mixtures, using the baseline technique. The chemical structures of ortho-
meta- and para-xylene are shown in Figure 2.

Figure 2: Chemical structures of ortho-, meta- and para- xylene

MATERIALS

Chemicals

Ortho-xylene

Meta-xylene

Para-xylene

Cyclohexane
Apparatus

Beaker (100 mL)

Micropipette

METHODOLOGY

PART A: Preparation of solutions.

1. Ortho-, meta-, and para-xylene were provided.

2. A series of standard solutions in 10 mL volumetric flask were prepared by the following
volume of isomers as depicted in the 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. Cyclohexane was added to the mark of each volumetric flask.

PART B: IR analysis.

1. The instrument was operated by lab assistant.

2. The infrared cell was handle carefully avoiding eye contact with water and the fingers.
3. Spectra of each solution was run from 2000 to 650 𝑐𝑚−1
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. A peak for each isomer was chosen from the spectra of the pure substance.
5. Po/P for the peak for each compound were measured by using the baseline method.
6. An unknown mixture obtained from the lab assistant was run using the baseline
method and Po/P for the three compounds were 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 (logPo/P) for xylene isomers.

o- xylene isomer

Solution % o-xylene Po P Log Po/P

I 2 99.88 97.75 9.36 x 10-3
II 2 99.63 97.75 8.27 x 10-3
III 2 99.50 99.13 3.99 x 10-3
IV 2 99.34 98.00 7.34 x 10-3
Unknown 99.10 90.50 3.94 x 10-2

m- xylene isomer

Solution % m-xylene Po P Log Po/P

I 1 99.75 99.00 3.28 x 10-3
II 2 99.75 98.25 6.58 x 10-3
III 3 99.88 98.00 8.25 x 10-3
IV 5 99.50 96.00 1.56 x 10-2
Unknown 97.00 87.50 4.48 x 10-2

p- xylene isomer

Solution % p-xylene Po P Log Po/P

I 5 99.75 97.00 1.21 x 10-2
II 3 99.75 98.13 7.11 x 10-3
III 2 99.69 98.63 4.64 x 10-3
IV 1 99.63 96.88 1.22 x 10-2
Unknown 97.50 96.75 3.35 x 10-3
Solution of 50% (vol/vol) o-xylene in cyclohexane
% o-xylene Po P logPo/P
50 98.00 90.00 0.0370

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

% m-xylene Po P logPo/P
50 99.25 84.25 0.0712

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

% p-xylene Po P logPo/P
50 98.25 81.50 0.0812
DISCUSSIONS

This experiment needs us to prepare solution of 50% (vol/vol) o-xylene in cyclohexane,

solution of 50% (vol/vol) m-xylene in cyclohexane, solution of 50% (vol/vol) p-xylene in
cyclohexane, Standard solutions I-IV, pure cyclohexane solvent and unknown solution. But, it
has been prepared by our lab assistant.

We run spectra on each of the solutions and from the spectra of the pure subtances, we
choose a peak of each isomer o-xylene, m-xylene, p-xylene. The information on the peak
which we got from the lab assistant, is used to measure the absorbance, log Po/P for the
standard solution of each sample. We analyse the data for each sample using baseline
method by referring the figure below.
CONCLUSIONS

- Samples for IR analysis are prepared by lab assistant.

- Po/P for every compounds is measured by using baseline method.
- IR analysis on aqueous solution are performed by lab assistant.

REFERENCES

Schwartz, L.M. “Advances in Acid-Base Gran Plot Technology,” J. Chem. Educ., 64, 947-950
(1987).

Jayson VedadLauren ReillyRuel Z. B. DesameroElmer-Rico E. Mojica. Quantitative Analysis

of Xylene Mixtures Using a Handheld Raman Spectrometer. 2018,,, 129-152. DOI:
10.1021/bk-2018-1305.ch008.

Christian, G.D., Analytical Chemistry, 6th edition. New Jersey. John Wiley, 2004.

QUESTIONS

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

- Correct wavelength of incident radiation. A molecules absorb radiation only when
the frequency of the incident radiation is equivalent to the natural frequency of
vibration of the part of the molecule. After absorption of the correct wavelength of
radiations, the molecule vibrates at increased amplitude due to absorbed IR
energy.
- There must be a change in the dipole moment of the molecule as a result of a
molecular vibration (or rotation). The change (or oscillation) in the dipole moment
allows interaction with the alternating electrical component of the IR radiation wave.
Symmetric molecules (or bonds) do not absorb IR radiation since there is no dipole
moment.
2. What types of molecular vibration are associated with infrared absorption?

1. Stretching vibrations

In this type of vibrations, the bond length is increased or decreased at regular intervals.
There are two types of stretching vibrations. Symmetrical stretching and asymmetrical
training.

Symmetrical stretching

- In this type of stretching, bond length increase or decrease symmetrically

Asymmetrical stretching

- In this type of stretching, length of one bond increases and the other one
decreases.

2. Bending vibrations

In this type of vibrations, a change in bond angle occurs between bonds with a common
atom, or there is a movement of a group of atoms with respect to the reminder of the
molecule without movement of the atoms in the group with respect to one another.
3. Define the following:
a) Chromophore
A chemical group that absorbs light at a specific frequency and so imparts
colour to a molecule.
b) Auxochrome
A group of atoms attached to a chromophore which modifies the ability of that
chromophore to absorb light. When attached to chromophore it alters both the
wavelength and intensity of absorption.
c) Bathocrhomic shift
A change of spectral bend position in the absorption, reflectance, transmittance
or emission spectrum of a molecule to a longer wavelength.
d) Hypsochromic shift
Denoting the shift of an absorption spectrum maximum to a shorter wavelength
(greater energy)
e) Hyperchromism
Increase of absorbance (optical density) of a material
f) Hypochromism
Decrease of absorbance is called hypochromicity

4. Sulfur dioxide is a nonlinear molecule. How many vibrational modes will this
compound have? How many absorption peaks would sulfur dioxide be expected
to have?
SO2 is a non-linear triatomic molecule.
Thus,
= 3N – 6

= 3(3) – 6

=3

Theoretically, SO2 has three vibrations modes, therefore three absorptions

peak.
5. What are the advantages of a Fourier transform infrared (FTIR) spectrometer
compared to a dispersive instrument?
- High sample throughput
- Improvement in sensitivity
- Increased energy throughput
- Low maintenance