DEPARTMENT OF CHEMICAL ENGINEERING,

UNIVERSITI TEKNOLOGI PETRONAS.

CDB 3093 : ANALYTICAL CHEMISTRY

Title : [Experiment] – Fourier Transformed Infrared Spectroscopy

Qualitative Analysis

Group : Table No 8

Group Members : Hirreish Rajendran 16001170

Sanjeev Nehru Jawahar Nehru 16001174

Dewiyaa Narayanan 16001555

Sujana Nair Wabalakersinan 16001504

Darshanasri Sivakumar 16000770

Lab Coordinator : Dr Dzul Hakim Wirzal

Ms Nur Farhana Ajua

Graduate Assistant : Ms Siri Munirah

th
Experiment Date : 18 June 2019
th
Submission Date : 19 June 2019

1
TABLE OF CONTENTS

1.0 OBJECTIVE………………………………………………………………………………………3

2.0 INTRODUCTION…………………………………………………………………………….......3

3.0 APPARATUS & MATERIALS…………………………………………………………4

4.0 METHODOLOGY……………………………………………………………………….4

5.0 RESULTS & DISCUSSION…………………………………………………………...5-7

6.0 QUESTIONS………………………………………………………………………….8-10

7.0 CONCLUSION………………………………………………………………………….11

8.0 REFERENCES…………………………………………………………………………12

9.0 APPENDICES………………………………………………………………………13-14

2
1.0 OBJECTIVE

To conduct an experiment using Fourier Transformed Infrared spectroscopy for 3 samples

which then allow us to identify the functional groups of membrane 10,13 and 6 which would
be use as fingerprint for respective membrane.

2.0 INTRODUCTION

As for this experiment, functional group of few samples given are determined by utilising an
instrumental method known as the FTIR or Fourier transform infrared spectroscopy. FTIR is
a device that uses an infrared radiation that is being passed through a sample at many
frequencies and measures the amount of radiation that is being absorbed or transmitted by the
sample. (Introduction to FTIR spectroscopy) This experiment is being conducted by using
FTIR-84002 Shimadzu model.
Upon having radiation being absorbed or transmitted, this infrared spectroscopy experience
signal at the detector which is a spectrum representing a molecular ‘fingerprint’ of the
respective samples. Fourier transformed infrared spectrophotometer is also applicable for
absorption or emission of solid, liquid and gas and is capable of simultaneously collect high
spectral resolution data over a wide spectral range.
In this experiment, the infrared radiation with wavelength of 700nm to 5000nm is being
found in the electromagnetic spectrum between the visible and microwave region. This
method can be applied to the analysis of organic molecules by causing molecular rotation or
molecular vibration (stretching and bending of bonds) in the molecules. Three samples were
given named 10,13 and 6 and we had to identify which functional groups are there in all three
samples.

3
3.0 APPARATUS & MATERIALS

APPARATUS
• Fourier Transform Infrared Spectrophotometer
MATERIALS
• Polystyrene Calibration Film
• 2 Membrane samples

4.0 METHODOLOGY

A. Obtaining IR Spectra
1. Three membrane samples were prepared and labelled as S2, S10 and S12.
2. S2 is placed in the sample holder and the spectrum is obtained.
3. Step 2 is repeated with S10 and S12.
4. Graph of transmission (%) versus wavelength (cm-1) were plotted for each samples.
5. The functional groups of the samples were determined based on the range of wavelength.

4
5.0 RESULTS & DISCUSSION

Sample 10

Sample 10
105

100

95
T%

90

85

80
2576
4000
3911
3822
3733
3644
3555
3466
3377
3288
3199
3110
3021
2932
2843
2754
2665

2487
2398
2309
2220
2131
2042
1953
1864
1775
1686
1597
1508
1419
1330
1241
1152
1063
974
885
796
707
618
Wavenumber cm-1

Figure 5.1: FTIR Spectra of Sample 10

Wavenumber(cm-1) Functional Group Type of Vibration Intensity

3296.29 O-H stretching Variable, sometimes

broad
2916.32 C-H stretching strong

2848.75 C-H stretching strong

1641.06 C=C stretching variable

1466.01 C-H bending strong

1081.45 C-O stretching strong

718.22 C-H bending strong

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Sample 13

Sample 13
104
102
100
98
96
T%

94
92
90
88
86
3090

1543
4000
3909
3818
3727
3636
3545
3454
3363
3272
3181

2999
2908
2817
2726
2635
2544
2453
2362
2271
2180
2089
1998
1907
1816
1725
1634

1452
1361
1270
1179
1088
997
906
815
724
633
Wavenumber cm-1

Figure 5.2: FTIR Spectra of Sample 13

Wavenumber (cm-1) Functional Group Type of Vibration Intensity

3025.43 C-H stretching medium

2922.38 C-H stretching strong
2852.46 C-H stretching strong
1744.27 C=O stretching strong
1600.77 C=C stretching variable

1492.46 C=C stretching variable

1451.13 C-H bending strong

1372.29 C-H bending strong

1154.52 C-O stretching strong

1027.45 C-O stretching strong

906.33 C-H bending strong

753.20 C-H bending strong

695.90 C-H bending strong

6
Sample 6

Sample 6
120

100

80
T%

60

40

20

0
3363

3090

1543
4000
3909
3818
3727
3636
3545
3454

3272
3181

2999
2908
2817
2726
2635
2544
2453
2362
2271
2180
2089
1998
1907
1816
1725
1634

1452
1361
1270
1179
1088
997
906
815
724
633
Wavenumber cm-1

Figure 5.3: FTIR Spectra of Sample 6

Wavenumber (cm-1) Functional Group Type of Vibration Intensity

2919.28 C-H stretching strong

1642.11 C=C stretching variable

1456.59 C-H bending strong

1376.20 C-H bending strong

1087.26 C-O stretching strong

607.09 C-H bending strong

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6.0 QUESTIONS

1. Explain the beer-Lambert law. How do you apply in FTIR for quantitative and
qualitative measurement?

The Beer-Lambert law is a linear relationship between absorbance and concentration

of an absorbing species. It relates the attenuation of light to properties of a material
where the quantity of light absorbed by a substance dissolved in a fully transmitting
solvent is directly proportional to the concentration of the substance and the path length
of the light through the solution. This law is applied to the analysis of a mixture by
spectrophotometry and it can be used to determine concentrations of a particular
substance or determine the molar absorptivity of a substance.

Figure 6.1: Formula of Beer-Lambert Law and the block diagram process

Figure 6.2: Formula of Absorbance and Transmittance

FTIR is applied effectively for quantitative measurement as non-destructive
measurement of samples is possible. Samples of known concentrations are prepared
and will be analyzed. By identifying the prominent IR peak in the sample, the
calibration curve can be plotted. Then, the concentration of the unknown sample can
be determined by taking note of the peak height.

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 FTIR can also be applied for qualitative measurement as this method is suitable for
solid, liquid or gases and is able to identify bulk materials. The composition of
materials is characterized, contamination in the sample are identified and the changes
seen in the sample are recorded as FTIR identifies chemical bonds in a molecule by
producing an infrared absorption spectrum. FTIR is also an effective analytical
instrument for detecting functional groups and characterizing covalent bonding
information.

2. Sketch the main components of an FTIR infared absorption spectrophotometer.

3. Hand in copies of all spectra acquired during this experiment.

Refer appendices.

4. Explain why the IR Background spectrum has peaks even though the sample
chamber was empty.

The IR background spectrum has peaks despite the sample chamber was empty due to
the presence of carbon dioxide and air which contains moisture that are detected by the
instrument. The sample chamber is not exactly empty but contains environment air in
it. Therefore, the spectrum shows peaks.

5. Examine the Polystyrene spectrum. Using the structure of Polystyrene, identify

the major peaks in the spectrum.

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 104
100

95
1744.27cm-1 1372.29cm-1 1154.52cm-1 906.33cm-1
90 3025.43cm-1 1600.77cm-1
1027.45cm-1
85 2852.46cm-1

1492.46cm-1
80 1451.13cm-1
2922.38cm-1

75
753.20cm-1
%T

70

65

60

55

50

45 695.90cm-1

39
4000 3500 3000 2500 2000 1500 1000 550
cm-1

Peak (cm-1) Functional Group Intensity

3025.43 C-H Medium
2922.38 C-H Strong
2852.46 C-H Strong
1744.27 C=O Strong
1600.77 C=C Variable
1492.46 C=C Variable
1451.13 C-H Strong
1372.29 C-H Strong
1154.52 C-O Strong
1027.45 C-O Strong
906.33 C-H Strong
753.20 C-H Strong
695.50 C-H Strong

6. Examine the Membrane 1 and Membrane 2. How do you distinguish between the
two membranes?
Membrane 1 contains 3 types of functional group such as alcohols, alkanes and
alkenes while Membrane 2 contains 2 types of functional group such as alkanes and
alkenes. Hence, these two membranes are distinguished based on their functional
group.

7. Discuss the possible sources of systematic and random errors in the above
experiments.
8. There are many possible sources of errors in this experiment. For systematic error, it
may have occurred due to the instrumentation error whereby small components such
as dust may be present and may cause inaccuracy of results in the instrument. To
improve accuracy of reading, the instrument should be inspected properly before
using it. For random error, it is related to human error as it is very difficult to evaluate
the peaks from the given results. Therefore, it increases the error and inaccuracy of
readings. To overcome this error, the unknown sample should be scanned multiple
times to make comparisons and have a clearer understanding on the results of the
experiment.

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7.0 CONCLUSION

To conclude, the FTIR experiment has fulfilled the main objective which is by identifying
the functional group of each samples that was examined and the use of fingerprint membrane
identification. Thus, samples of 6, 10 and 13 was used throughout the experiment.

Based on the results, sample 6 shows the functional groups of C-H, C=C and C-O, sample
10 shows the functional groups of O-H, C-H, C=C and C-O, whereas sample 13 shows the
functional groups of C-H, C=O, C=C and C-O.

In summary, the FTIR unit can only detect the functional group of the samples but
cannot determine the molecular weight of the samples. Thus, to determine the molecular
weight of the sample tested, identifying the functional group detected by the unit on the
sample should be carried out significantly

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8.0 REFERENCES

Introduction to FTIR spectroscopy. (n.d.). Retrieved from ThermoFisher Scientific:

https://www.thermofisher.com/my/en/home/industrial/spectroscopy-elemental-isotope-
analysis/spectroscopy-elemental-isotope-analysis-learning-center/molecular-spectroscopy-
information/ftir-information/ftir-basics.html

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9.0 APPENDICES

SAMPLE 1
103
102

100

3296.29cm-1
98

1641.06cm-1
96 718.22cm-1
%T

1466.01cm-1
94 1081.45cm-1

92

90 2848.75cm -1

88 2916.32cm-1
87
4000 3500 3000 2500 2000 1500 1000 550
cm-1

Sample Name Description Saved or unsaved Spectrum quality

State check summary
group 8 s10 Sample 1266 By Saved The Quality Checks
Administrator Date give rise to a Weak
Tuesday, June 18 2019 Bands warning for the
sample.

SAMPLE 2
102

101

100

99
607.09cm-1

98

97
1642.11cm-1
%T

96
1087.26cm-1
95
1456.59cm-1

94
2919.28cm-1 1376.20cm-1
93

92
91
4000 3500 3000 2500 2000 1500 1000 550
cm-1

Sample Name Description Saved or unsaved Spectrum quality

State check summary
group 8 sample 13 Sample 1267 By Saved The Quality Checks
Administrator Date give rise to a Weak
Tuesday, June 18 2019 Bands warning for the
sample.

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SAMPLE 3
104
100

95
1744.27cm-1 1372.29cm-1 1154.52cm-1 906.33cm-1
90 3025.43cm-1 1600.77cm-1
1027.45cm-1
85 2852.46cm-1

1492.46cm-1
80 1451.13cm-1
2922.38cm-1

75
753.20cm-1
%T

70

65

60

55

50

45 695.90cm-1

39
4000 3500 3000 2500 2000 1500 1000 550
cm-1

Sample Name Description Saved or unsaved Spectrum quality

State check summary
group 8 sample 6 Sample 1268 By Saved The Quality Checks do
Administrator Date not report any
Tuesday, June 18 2019 warnings for the
sample.

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