EXPERIMENT 5: ANALYSIS OF ASCORBIC ACID IN COMMERCIAL VITAMIN C TABLET

USING FTIR

OBJECTIVES

To determine ascorbic acid content in vitamin C tablet.

INTRODUCTION

FTIR relies on the fact that the most molecules absorb light in the infra-red region of
the electromagnetic spectrum. This absorption corresponds specifically to the bonds present
in the molecule. The frequency range are measured as wave numbers typically over the range
4000 – 600 cm-1. The background emission spectrum of the IR source is first recorded, followed
by the emission spectrum of the IR source with the sample in place. The ratio of the sample
spectrum to the background spectrum is directly related to the sample's absorption spectrum.
The resultant absorption spectrum from the bond natural vibration frequencies indicates the
presence of various chemical bonds and functional groups present in the sample. FTIR is
particularly useful for identification of organic molecular groups and compounds due to the
range of functional groups, side chains and cross-links involved, all of which will have
characteristic vibrational frequencies in the infra-red range.

A common FTIR spectrometer consists of a source, interferometer, sample

compartment, detector, amplifier, A/D convertor, and a computer. The source generates
radiation which passes the sample through the interferometer and reaches the detector. Then
the signal is amplified and converted to digital signal by the amplifier and analog-to-digital
converter, respectively. Eventually, the signal is transferred to a computer in which Fourier
transform is carried out.
 Ascorbic acid

Ascorbic acid (vitamin C) is used to prevent or treat low levels of vitamin C in people
who do not get enough of the vitamin from their diets. Most people who eat a normal diet do
not need extra ascorbic acid. Low levels of vitamin C can result in a condition called scurvy.
Scurvy may cause symptoms such as rash, muscle weakness, joint pain, tiredness, or tooth
loss. Vitamin C plays an important role in the body. It is needed to maintain the health of skin,
cartilage, teeth, bone, and blood vessels. It is also used to protect your body's cells from
damage. It is known as an antioxidant.

INSTRUMENT

Instrument Model: Perkin Elmer – Spectrum One (FTIR)

APPARATUS

Beakers, volumetric flask and pipette.

SAMPLE

Vitamin C tablet
PROCEDURE

a) Sample Preparation

i. Mixture of sample and KBr

The agate mortar and pestle are removed from the desiccators. 0.001 g sample is
grinded in agate mortar into powder. 0.080 g KBr is added into the sample powder.
They are mixed using the pestle. The mixture is scrapped and heaped in the centre
of the mortar and is grinded again for 1 minute. The KBr is kept back into the
desiccators after used.

ii. KBr pellets

Transfer one fourth of the KBr mixture into the collar of the hand press. The anvil is
placed along with the longer die pin so that is comes into contact with the samples.
The die set is carefully lifted by holding the lower anvil. The collar is make sure
stayed in place. The handle of the hand press is opened slowly and the die set is
inserted into the hand press. The handle is closed. The dial pressure is rotated until
the upper ram of the hand press slightly touched the upper anvil on the die assembly.
The unit is tilted back in order to hold the die set from falling off. The handle is
opened. The pressure dial is rotated clockwise in one half turn. The mixture is
compress slowly while closing the handle in 2 minutes. The unit is tilted back, the
handle is opened and the die set is removed from the unit carefully. The pellet is
weighted and inspected. The samples are ready for the analysis. An IR spectrum is
obtained.

RESULT

Functional groups Wavenumber (cm-1)

Hydroxyl (OH) 2849.80, 2918.20, 3414.94

Carbon-Carbon double bond (C=C) 1658.43

Carbonyl (C=O) 1691.51

DISCUSSION

The purpose of this experiment is to determine ascorbic acid content in vitamin C tablet
by using FTIR. IR radiation does not have enough energy to induce electronic transitions as
seen in UV. Absorption of IR is restricted to compounds with small energy differences in the
possible vibrational and rotational states. For a molecule to absorb IR, the vibrations or
rotations within a molecule must cause a net change in the dipole moment of the molecule.
The alternating electrical field of the radiation (electromagnetic radiation consists of an
oscillating electrical field and an oscillating magnetic field, perpendicular to each other)
interacts with fluctuations in the dipole moment of the molecule. If the frequency of the radiation
matches the vibrational frequency of the molecule then radiation will be absorbed, causing a
change in the amplitude of molecular vibration. Certain gases in the atmosphere have the
property of absorbing infrared radiation. Oxygen and nitrogen the major gases in the
atmosphere do not have this property. This is because, there will only be IR absorption if the
value and direction of the molecular dipole moment changes during the vibration. Since O2 is
a diatomic molecule consisting of two of the same atoms, there is no dipole moment at all and
it therefore won't have any IR absorption.

A machine called an IR spectrometer passes infrared radiation through a sample of an

unknown compound and uses a detector to plot percent transmission of the radiation through
the molecule versus wavenumber of the radiation. A downward peak on the plot represents
absorption at a specific wavenumber. In sum, IR spectroscopy is useful in determining
chemical structure because energy that corresponds to specific values allows us to identify
various functional groups within a molecule. When infrared light of the same energy as a
vibrational transition impinges upon a molecule, the energy may be absorbed. The
corresponding decrease in light energy at the absorption wavenumber gives rise to a peak in
the measured infrared spectrum of the molecule. The peak positions in an infrared spectrum
thus disclose the vibrational energy levels of the functional groups in a molecule, and when
infrared spectra are analysed, the peaks are assigned to specific vibrations of specific
functional groups.

Thus, infrared spectroscopy is a type of functional group spectroscopy, and infrared

spectrometers are used to detect functional groups. The peak positions in an infrared spectrum
are used to distinguish different functional groups from each other. Different functional groups
can have peaks at about the same position. The peaks of different functional groups can be
distinguished from each other by using the peak heights and peak widths information. Different
functional groups have different peak intensities and peak widths. By integrating the peak
position, height, and width information in a spectrum will be more successful at interpreting
spectra than just using the peak positions by themselves.

The three prominent peaks from the obtained spectrum are hydroxyl groups (OH) from
2849.80 to 3414.94 cm-1, carbon to carbon double bond (C=C) at 1658.43 cm-1 and carbonyl
group for ester (C=O) at 1691.51 cm-1. The similarity matching of the ascorbic acid in KBr
spectrum in vitamin C tablet with the pure ascorbic acid from literature is 44.06 %. This
percentage of match is considered low because the exact value must be around 90 % and
above. We could not obtain that value since the vitamin C tablet that is used that day has
expired for too long. Thus, the content of ascorbic acid might have reduced from the original
content.

A common FTIR spectrometer consists of a source, interferometer, sample

compartment, detector, amplifier, A/D convertor, and a computer. The source generates
radiation which passes the sample through the interferometer and reaches the detector. Then
the signal is amplified and converted to digital signal by the amplifier and analog-to-digital
converter, respectively. Eventually, the signal is transferred to a computer in which Fourier
transform is carried out. The interferogram is a function of time and the values outputted by
this function of time are said to make up the time domain. The time domain is Fourier
transformed to get a frequency domain, which is deconvolved to product a spectrum. The
interferogram obtained is a plot of the intensity of signal versus OPD. A Fourier transform can
be viewed as the inversion of the independent variable of a function. Thus, Fourier transform
of the interferogram can be viewed as the inversion of OPD. The unit of OPD is centimetre, so
the inversion of OPD has a unit of inverse centimetres, cm-1. Inverse centimetres are also
known as wavenumbers. After the Fourier transform, a plot of intensity of signal versus
wavenumber is produced. Such a plot is an IR spectrum.

CONCLUSION

In conclusion, the amount of ascorbic acid in vitamin C tablet obtained by using FTR
is 44.06 % match with the pure ascorbic acid from literature.
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https://chem.libretexts.org/Core/Physical_and_Theoretical_Chemistry/Spectroscopy/Vibr
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Charles, E. (2003). Greenhouse Gases Absorb Infrared Radiation. Retrieved on December 8,

2017 from http://chemistry.elmhurst.edu/vchembook/globalwarmA5.html

WebMD. (n.d.). Ascorbic Acid. Retrieved on December 8, 2017 from

https://www.webmd.com/drugs/2/drug-322/ascorbic-acid-vitamin-c-oral/details