ejbps, 2015, Volume 2, Issue 3, 490-497.

Valli et al.

Research Article

SJIF Impact Factor 2.062

2349-8870
European
Journal ofof
Biomedical
and PharmaceuticalISSN
Sciences
European
Journal
Biomedical
Volume: 2
AND
Issue: 3
490-497
Pharmaceutical sciences
Year: 2015

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A GREEN METHOD FOR THE SYNTHESIS OF TITANIUM DIOXIDE

NANOPARTICLES USING CASSIA AURICULATA LEAVES
EXTRACT
Dr. G. Valli*1 and S. Geetha2
*1Associate Professor & Head, 2M.Phil Scholar, Department of Chemistry, S.F.R. College,
Sivakasi -626123, Virudhunagar District, Tamilnadu.
Article Received on 13/04/2015

*Correspondence for

Article Revised on 04/05/2015

Article Accepted on 25/05/2015

ABSTRACT

Author

Knowing the importance of titanium dioxide nanoparticles and Cassia

Dr. G. Valli

auriculata as revealed by various literature resources, Green synthesis

Associate Professor & Head

of titanium dioxide nanoparticles using Cassia auriculata leaves were

Department of Chemistry,
S.F.R. College, Sivakasi 626123, Virudhunagar
District, Tamilnadu.

carried out. The formation of titanium dioxide nanoparticles were

identified first by observing the color changes of the extract. Secondly
titanium dioxide nanoparticles were confirmed by the spectral studies
like UV-Visible, FT-IR, X-Ray Diffraction and Field Emission

Scanning ElectronMicroscopy. UV absorbance at 447.3 nm and M-O stretching at 516.92

cm-1 by FT-IR for the TiO2 nanoparticles were observed. XRD and FE-SEM analysis of TiO2
nanoparticles showed that they were found to exhibit spherical shape with an average size of
38.0 nm.
KEYWORDS: Cassia auriculata, UV-Vis, FT-IR, XRD and FE-SEM.
INTRODUCTION
Cassia auriculata Linn (Family: Caesalpiniaceae) commonly known as Tanners senna, is
distributed throughout hot deciduous forests of India and holds a very prestigious position in
Ayurveda and Siddha systems of medicine. It was profoundly used in ayurvedic medicine as
a tonic, astringent and as a remedy for diabetes, conjunctivitis and opthalmia.[1] Cassia
auriculata have been shown to possess antibacterial, antifungal, antiprotozoal, antipyretic[2],
hepatoprotective[3],

antidiabetic,

antiperoxidative

and

antihyperglyceamic[4],

antimicrobicidal[5] and antihyperlipidaemic activities.[6] The flowers are used to treat urinary

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discharges, nocturnal emissions, diabetes and throat irritation.[7] They are one of the
constituent of polyherbal formulation Diasulin in the concentration range of 40 mg/dl which
is proven to have antidiabetic activity.[8] Cassia auriculata medicinal properties are due
mainly to the content of hydroxyanthraquinone derivative. The uses of Cassia auriculata plant
bio-active compounds for pharmaceutical purpose have been gradually increased.[9] Titanium
dioxide (TiO2) is thermally stable, non-flammable, poorly soluble and it occurs in nature as
well-known minerals rutile, anatase and brookite.[10] The most important application areas are
paints and varnishes as well as paper and plastics, which account for about 80% of the
world's titanium dioxide consumption. Titanium dioxide is also used as a material in the
memristor, which can be employed for solar energy conversion based on Titanium dioxide
solar cells using conjugated polymers as solid electrolytes.[11] Synthetic single crystals and
films of Titanium dioxide are used as a semiconductor.[12] A significant amount of research
on TiO2 have been performed over the last five decades and a number of reviews on various
aspects of TiO2 have been published[13-18] to understand and summarize the progress in this
field. The properties of TiO2 that make it suitable to act as a photo catalyst and various
methods including dye sensitization, doping, coupling and capping are used to improve its
efficiency.
Knowing the importance of Cassia auriculata leaves extract and titanium dioxide nano
particles biological importance, a green method for the synthesis of titanium dioxide
nanoparticles using cassia auriculata leaves extract was performed.
MATERIALS AND METHODS
a) Materials
Cassia auriculata leaves (collected from the Jameen Nathampatti village, Rajapalayam,
virudhunagar district), titanium tetra isopropoxide and ethanol were used.
b) Methods
i) Preparation of Cassia Auriculata Leaves in Ethanol Extract
Dried leaves of Cassia auriculata were grinded to fine powder. The ethanol extract was
prepared by refluxing 15gm of leave powder and 150ml of ethanol solution by using soxhlet
apparatus to maintain carefully the temperature level at 50 600C for 3 hours. Then, the
extracts were collected in an airtight bottle and were kept in deep freezer for further use.

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ii) Synthesis of TiO2 Nanoparticles from Leaves Extract

For the synthesis of titanium dioxide nanoparticles, the Erylenmeyar flask containing 50 ml
of Cassia auriculata ethanol leaves extract, 50 ml of double distilled water were added to 0.4
ml of titanium tetra isopropoxide and subjected to under stirring at 500C. After four hours of
continuous stirring, the formed TiO2 nanoparticle was acquired by centrifugation at 10000
rpm for 15 minutes. Then the centrifuged particles were washed with ethanol and again
subjected to centrifugation at 5000 rpm for 10 minutes. Separated titanium dioxide
nanoparticles were grinded and calcinate at 5000C in muffle furnace for about 2 hours. The
calcined titanium dioxide nanopowder was used for further analytical characterization.
iii) Characterization of Titanium dioxide nanoparticles
a)UV- Visible Spectrophotometer Analysis:
The UV-DRS spectrum was recorded in Shimadzu UV- 2400PC series. Absorption spectra
of titanium dioxide nanoparticles(Figure-1) have absorbance peak at 447.3 nm.

.
Figure-1: UV-Visible Spectrum of TiO2 Nanoparticles
b) Fourier Transform - Infrared Spectroscopy
The FT-IR spectrum was recorded in Shimadzu FT-IR spectrometers 7600 and the
measurement of the samples were performed in transmission mode. In order to identity the
binding groups of the plant extract with titanium dioxide, FT-IR spectra of Cassia auriculata
leaves extract (Figure-2) and titanium dioxide nanoparticles (Figure-3) were recorded.

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Figure-2: FT-IR Spectrum of Cassia Auriculata leaves extract

Figure-3: FT-IR Spectrum of TiO2 Nanoparticles

c) X-Ray Diffraction Analysis
For the XRD (BRUKER ECO D8 ADVANCE) spectral analysis, prepared particles in
solution was purified by centrifugation at 5000 rpm for 20 minutes. An XRD spectrum was
recorded at Kalasalingam University and the spectra was given as Figure-4. The dried
mixture of titanium dioxide nanoparticles collected for the formation of titanium dioxide
nanoparticles by X-ray diffractometer operated at a voltage of 40 kV and a current of 20 mA
with Cu K radiation in -2 configuration. Morphology of the interplannar distance spacing
was calculated using Braggs equation.(n = 2d sin ).

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Figure-4: XRD Spectrum of TiO2 Nanoparticles

d) Field Emission Scanning Electron Microscopy
FE-SEM images of the green synthesized titanium dioxide nanoparticles obtained using
Cassia auriculata leaves extract recorded at Sastra University was shown in Figure-5.
The titanium dioxide nanoparticles exhibit good uniformity with the average diameter of
about38nm. The titanium dioxide nanoparticles sizes were found in the range 38.0 44.2
nm.

Figure-5: FE-SEM images of TiO2 Nanoparticles

RESULT AND DISCUSSION
Green synthesis of titanium dioxide nanoparticles using Cassia Auriculata leaves extract was
first identified by color changes of the extract. Secondly titanium dioxide nanoparticles were
confirmed by the spectral studies of UV-Visible Spectroscopy, FT-IR Spectroscopy, X-Ray
Diffraction and Field Emission Scanning Electron Microscopy.

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a) Ultraviolet Visible Spectrophotometer Analysis (UV-DRS)

UV-Visible Spectroscopy could be used to examine formation of titanium dioxide
nanoparticles. Absorption spectra of titanium dioxide nanoparticles formed in the reaction
media have shown the absorbance peak at 447.3 nm.
b) Fourier Transform - Infrared Spectroscopy Analysis (FT-IR)
On comparing the FT-IR spectra of Cassia auriculata leave extract (Figure-2) and the
titanium dioxide nanoparticles (Figure-3) revealed the following observation. The FT-IR
spectra of Cassia auriculata leave extract showed a broad band at 3317 cm-1 indicating the
presence of bonded OH group. Stretching at 1643 cm-1 indicated the presence of >C=O
group. The FT-IR spectra of titanium dioxide nanoparticles showed the following stretching
frequencies.
(i) at 1606 cm-1 (diminished carbonyl stretching)
(ii) 516.92 cm-1 (due to formation of Ti-O bond)
On comparing the IR spectra of both the extract and its assisted titanium dioxide
nanoparticles formation revealed the following observation. During the formation of titanium
dioxide nanoparticles assisted by Cassia Auriculata, the O-H bonds present in the extract
(observed by 3317 cm-1) diminishes that showed that O-H group, Oxygen may binds to
titanium dioxide in titanium dioxide nanoparticles. >C=O stretching frequency at 1643 cm-1
of the extract shifted to 1606 cm-1 in titanium dioxide nanoparticles that showed that carbonyl
oxygen enter into the binding with titanium dioxide nanoparticles. M-O stretching at 516.92
cm-1 also confirms the existence of Ti-O bond. Hence these observations indicated the
formation of titanium dioxide nanoparticles in which Ti binds strongly to the oxygen atom
present in the phytoconstituents of Cassia Auriculata extract.
c) X-Ray Diffraction (XRD)
Titanium dioxide nanostructures were confirmed by the characteristic peaks observed in the
XRD pattern. The analysis was carried out 2 value ranging from 100 to 900, with step size
0.020. All diffraction peaks correspond to the characteristic face centered cubic observed at
2 angle at 21.30, 31.50, 39.90, 430, 46.30, 640 and 75.90 respectively. Morphology of the
interplannar distance spacing was calculated using Braggs equation (n =2dSin).

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d) Field Emission Scanning Electron Microscope (FE-SEM)

FE-SEM observation of titanium dioxide nanoparticles proved that the average size was from
38.0 - 44.2 nm. (as given in Figure-5). However, further observation with high magnification
revealed that these TiO2 nanoclusters were assembled by smaller nanoparticles, which exhibit
good uniformity and the average diameter was about 38.0 nm.
CONCLUSION
Green synthesis of titanium dioxide nanoparticles using Cassia auriculata leaves extract
revealed the following observation. Formation of titanium dioxide nanoparticles was
confirmed by color changes of Cassia auriculata leaves extract and then characterized by UVVis, FT-IR spectral studies and their structure and size by XRD and FE-SEM analysis. UV
absorption studies of titanium dioxide nanoparticles showed the absorbance at 447.3 nm and
FT-IR studies showed the stretching frequency of M-O bond at 516.92 cm-1. Titanium
dioxide nanostructure was confirmed by the characteristic peaks observed in the XRD
pattern. All diffraction peaks correspond to the characteristic face centered cubic observed at
2 angle at 21.30, 31.50, 39.90, 430, 46.30, 640 and 75.90 respectively. FE-SEM observation
with high magnification reveals that these TiO2 nanoparticles were found to have an average
diameter about 38.0 nm.
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