ABSTRACT:

The Semiconductor Quantum Dots has increasing research attention

due to potential application such as quantum computing, single-electron
transistors, solar cells, LEDs, lasers, single-photon sources, second-harmonic
generation, quantum computing, and medical imaging. The main Advantage of
metal-semiconductor core-shell nanocrystals is the presence of the metal-
semiconductor interface that promotes effective charge carrier transfers to favor
charge separation and photocatalysis. The Cadmium Sulphide (CdS)
Semiconductor shell can protect the Au metal core from chemical poisoning.
Metals usually suffer from much serious oxidation since they have higher
oxidation potentials. Doping metals into semiconductors could eliminate the
chemical poisoning and extends the lifetime of the metal-semiconductor
composite nanocrystals during their photocatalytic operation. The Gold Quantum
dots can be synthesized by reducing gold chloride by using Green Extracts of
Ocimum sanctum (tulsi) and Punica granatum (Pomegranate). The unique
property of Gold Quantum dots is Surface Plasmon Resonance which leads to
high sensitivity in chemical sensing. CdS Quantum Dots can be synthesized by
hydrothermal reaction. Gold (Au) and CdS Quantum Dots can be coupled with
L-Cysteine to form Au-L-Cys-CdS and the hydrothermal reaction takes place at
130ºC decomposes L-Cysteine to yield Au-CdS Quantum Dots. Au-CdS
Quantum Dots exhibit phenomenon of fluorescent quenching and can be used in
sensing of heavy metal ions. The Au-CdS Quantum Dots can also be used for
photocatalytic degradation of Dyes. The Au-CdS Quantum Dots are also being
used to enhance the performance of electrochemical sensors for use in
environmental pollutants screens due to their Catalytic properties.
Keywords: Au-CdS Quantum Dots, fluorescent quenching, photocatalytic
degradation, electrochemical sensor.

1
 1. INTRODUCTION
Gold nanoparticles plays a important and frequent tool in nanotechnology, mainly
due to their surface plasmon resonance (SPR), their easy surface functionalization
and their chemical stability and biocompatibility. The size, concentration, and, in
some cases, aggregation level of Gold nanoparticles are key points for their
applications because they determine optical, electrical, chemical and biological
properties.
Integration of green chemistry principles to nanotechnology is one of the key
issues of nanoscience research. Cross-disciplinary nanoscience research
involving chemists, physicists, biologists and engineers is concerned about the
need for developing environmentally friendly and sustainable methods for the
synthesis of nanomaterials. Currently, there is a growing need to develop
environmentally benign metal nanoparticle synthesis processes that do not use
toxic chemicals in the synthesis protocols to avoid adverse effects in medical
applications. Gold nanoparticles can be used in medical science for bio-labeling
and detecting various ailments and in biosensor devices for the detection of
viruses and bacteria. Silver nanoparticles have received attention due to its
antibacterial properties. Physical and chemical methods of nanoparticle synthesis
are not environmentally friendly. Natural environment is a rich source of crude
untreated extracts of plants, marine organisms and microorganisms and it is
crucial to investigate their various properties. Biosynthesis of metal nanoparticles
using natural products is now an emerging area of nanoscience research.
Semiconductor, magnetite, or metal-based composite nanocrystals have attracted
increasing research attention in recent years for their possible improvement in
optical, electronic, magnetic, and catalytic functionalities. In particular, great
progress has been made in creating core-shell hetero structures by assembling
both metal and semiconductor nanocrystals. Such metal/semiconductor
combination is of particular interest to photocatalytic5 and electron storage
applications.6 For metal semiconductor core-shell nanocrystals, the presence of
the metal-semiconductor interface may promote effective charge carrier transfers
to favor charge separation and subsequent photocatalysis.7 In addition, the
semiconductor shell can protect the metal core from chemical poisoning (the
hole- or hydroxyl radical-mediated oxidation decomposition) as exposed to the
surrounding medium.8 Metals usually suffer from much serious oxidation since
they possess higher oxidation potentials. Embedding metals into semiconductors
could reasonably alleviate the chemical poisoning and thus extend the lifetime of
the metal/ semiconductor composite nanocrystals during their photocatalytic
operation.

2
OBJECTIVE OF THE PROJECT:
 Green Synthesis of Gold Nanoparticles and hydrothermal synthesis of
(Cadmium Sulphide) CdS and Au-CdS Quantum Dots.
 Characterisation of prepared Sample.
 Study on Degradation of Organic pollutants.
METHODOLOGY:
 SYNTHESIS OF GOLD NANO PARTICLES
Gold Nanoparticles are synthesised from extracts of Tulsi (Ocimum sanctum) and
Pomogranate (Punica granatum).
 SYNTHESIS OF CdS QUANTUM DOTS
CdS Quantum Dots are prepared by using Cadmium acetate and L-cysteine by
using Hydrothermal Method.
 SYNTHESIS OF Au-CdS QUANTUM DOTS
Au-CdS Quantum Dots are synthesised by using L-cysteine. The hydrothermal
Reaction taking place at 130ºC decomposes cysteine to Au-CdS Quantum Dots.
PROBLEM FACED:
Persistent organic pollutants (POPs), sometimes known as "forever chemicals"
are organic compounds that are resistant to environmental degradation through
chemical, biological, and photolytic processes. These Organic Pollutants bio-
accumulate with potential adverse impacts on human health and the environment.
There is a need to develop a new material to degrade the organic pollutant present
in environment.
SCOPE OF THE PROJECT:
Nanomaterial and Quantum dots are rapidly developing Technology and we used
this technology to degrade organic pollutants. We used both green Chemistry and
Chemical methods in our project. The Quantum dots has wide applications and
the quantum dots can be potentially harnessed in environmental clean-up
application.

3
 2. LITERATURE REVIEW

1. Bodunov, E. N., & Simões Gamboa, A. L. (2018). “Kinetics of

photoluminescence decay of colloidal quantum dots: Nonexponential
behavior and detrapping of charge carriers”, The Journal of Physical
Chemistry C, 122(19), 10637-10642. (New function for the description of the
whole PL decay curves of drop-cast films of CdSe/ZnS QDs at room temperature
is proposed whose parameters have a straightforward physical meaning,
accounting for the long-time tails of the decays and highlighting the role of
detrapping of charge carriers. This function and the interpretation of thePL decay
that it provides represent an alternative to the widespread assumption that Förster
resonance energy transfer takes place in systems of densely packed nearly
monodisperse colloidal QDs.)
2. Pandi, D. V., Muthukumarasamy, N., Agilan, S., & Velauthapillai, D. (2018).
CdSe quantum dots sensitized ZnO nanorods for solar cell application.
Materials Letters, 223, 227-230. Sol gel dip coating method has been used for
preparing ZnO nanorods. ZnO nanorods have been sensitized using CdSe
quantum dots by simple chemical method. Uniform coverage of quantum dots on
ZnO nanorods is observed. The structural, optical and morphology of the ZnO
nanorods, CdSe quantum dots and CdSe quantum dot sensitized ZnO nanorods
have been studied. The presence of CdSe quantum dots in ZnO nanorods based
film is clearly seen in FESEM and TEM image and the elements Zn, O, Cd and
Se present in the film was confirmed by EDAX analysis.
3. Yulizar, Y., Utari, T., Ariyanta, H. A., & Maulina, D. (2017). Green method
for synthesis of gold nanoparticles using polyscias scutellaria leaf extract
under uv light and their catalytic activity to reduce methylene blue. Journal
of Nanomaterials, 2017. The AuNPs have a size of 5–20 nm and have a face
centered cubic (fcc) crystal structure and are stable for 21 days. Phenolic
compounds, which are secondarymetabolites of PSE, act as an active compound
to reduce Au3+ ion to Au0, as well as stabilize the AuNPs through their surface
interaction with carbonyl and hydroxyl groups of phenols. AuNPs exhibit
excellent catalytic activity for the reduction of methylene blue with NaBH 4.The
reduction of methylene blue using AuNPs catalysts is a pseudo-first-order
reaction with a reduction rate constant (𝑘 obs) of 0.0223 min−1.
4. Chairam, S., Konkamdee, W., & Parakhun, R. (2017), Starch-supported gold
nanoparticles and their use in 4-nitrophenol reduction, Journal of Saudi
Chemical Society, 21(6), 656-663.(Gold nanoparticles have been synthesized

4
through a green synthesis method using mung bean starch as both reducing and
stabilizing agents. The chemical state was analyzed by X-ray photoelectron
spectroscopy.)
5. Peng, X., Long, Q., Li, H., Zhang, Y., & Yao, S. (2015)., “Turn on-off”
fluorescent sensor for protamine and heparin based on label-free silicon
quantum dots coupled with gold nanoparticles.(Sensors and Actuators B:
Chemical, 213, 131-138. An ultrasensitive “turn on-off” fluorescent sensor was
presented for determination of protamine andheparin based on the high quenching
ability of gold nanoparticles (AuNPs) to the fluorescence of siliconquantum dots
(SiQDs) as well as high binding affinity of protamine with heparin. The
fluorescence ofSiQDs was quenched significantly by adding AuNPs into SiQDs
solution.)
7. Kumar, B., Smita, K., & Cumbal, L. (2015),Phytosynthesis of gold
nanoparticles using Andean Ajı′(Capsicum baccatum L.),Cogent Chemistry,
1(1), 1120982. (AuNPs were characterized using Transmission electron
microscopy, Dynamic Light Scattering, and X-ray diffraction. It produced
spherical AuNPs at λmax = 540 nm of average size 23.9 ± 9.7 nm without any
aggregation. Ajı′ extract (aq) was the good reducing and capping agent in terms
of conversion to Au3+ to AuNPs. The synthesized AuNPs, also enhancing the
photocatalytic degradation of methylene blue (>50%, k = 1.9585 × 10−3 min −1)
under direct solar light irradiation.)
8. Ju, J., & Chen, W. (2015),In situ growth of surfactant-free gold
nanoparticles on nitrogen-doped graphene quantum dots for
electrochemical detection of hydrogen peroxide in biological environments,
Analytical chemistry, 87(3), 1903-1910. (The formation of hybrid was achieved
by just mixing the N-GQDs and HAuCl4·4H2O without addition of any other
reductant and surfactant. High resolution transmission electron microscopy
(HRTEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy
(XPS) characterizations clearly showed the formation of Au nanoparticles with
predominantly exposed (111) facets which can provide more adsorption sites.)
9. Herizchi, R., Abbasi, E., Milani, M., & Akbarzadeh, A. (2016),Current
methods for synthesis of gold nanoparticles. Artificial cells, nanomedicine,
and biotechnology, 44(2), 596-602. (Gold nanoparticles (GNPs), in particular,
are very attractive because of their size and shape-dependent properties.Metal
nanoparticles have gathered extensive attention due to their uncommon properties
and promising applications in photonics, electronics, biochemical sensing, and
imaging.)

5
10. Nadagouda, M. N., Iyanna, N., Lalley, J., Han, C., Dionysiou, D. D., &
Varma, R. S. (2014), “Synthesis of silver and gold nanoparticles using
antioxidants from blackberry, blueberry, pomegranate, and turmeric
extracts”, ACS Sustainable Chemistry & Engineering, 2(7), 1717-1723. (Greener
synthesis of Ag and Au nanoparticles is described using antioxidants from
blackberry, blueberry, pomegranate, and turmeric extracts. The synthesized
particles were characterized using X-ray diffraction (XRD), transmission electron
microscopy (TEM), high resolution TEM (HR-TEM), particle size analysis, UV-
Vis spectroscopy and thermo-gravimetric analysis.)
11. Veeraanga, M. S. P. K., & Ramasamy, P. (2014),“Synthesis and
characterization of cadmium sulfide (CdS) quantum dots (QDs) for
quantum dot sensitized solar cell applications, Int. J. Chem. Tech. Res, 6, 5396-
9. (Cadmium sulfide (CdS) quantum dots were prepared at various time durations
and deposited by chemical bath deposition (CBD) method. The structural,
morphological and optical properties were studied using powder X-ray diffraction
(PXRD), scanning electron microscope (SEM) and UV-Vis NIR analysis
respectively.)
12. Ben‐Shahar, Y., Scotognella, F., Waiskopf, N., Kriegel, I., Dal Conte, S.,
Cerullo, G., & Banin, U. (2015),Effect of surface coating on the photocatalytic
function of hybrid CdS–Au nanorods,Small, 11(4), 462-471. (The effects of
the surface coatings on the photocatalytic function are studied, with Au-tipped
CdS nanorods as a model hybrid nanoparticle system. Kinetic measurements of
the hydrogen evolution rate following photocatalytic water reduction are
performed on similar nanoparticles but with different surface coatings, including
various types of thiolated alkyl ligands and different polymer coatings.)
13. Rao, A., Mahajan, K., Bankar, A., Srikanth, R., Kumar, A. R., Gosavi, S., &
Zinjarde, S. (2013),Facile synthesis of size-tunable gold nanoparticles by
pomegranate (Punica granatum) leaf extract: Applications in arsenate
sensing,Materials Research Bulletin, 48(3), 1166-1173. (Gallic acid in the
extract mediated the reduction and a natural decapeptide capped the
nanostructures. Blocking of thiol groups in the decapeptide cysteine residues
caused the nanoparticles to aggregate. On interaction with arsenate (V) ions, the
UV–vis spectra of the nanoparticles showed a decrease in intensity and a red-
shift. Energy dispersive spectra confirmed the presence of arsenate associated
with the AuNPs.)
14. Sreelakshmi, C., Goel, N., Datta, K. K. R., Addlagatta, A., Ummanni, R., &
Reddy, B. V. (2013),Green synthesis of curcumin capped gold nanoparticles
and evaluation of their cytotoxicity, Nanoscience and Nanotechnology Letters,

6
5(12), 1258-1265.(The gold nanoparticle curcumin hybrids show long term
colloidal stability. Furthermore we evaluate the cytotoxic behaviour of curcumin
glycoside-Au nanoparticles.)
15. Mallikarjuna, K., Narasimha, G., Dillip, G. R., Praveen, B., Shreedhar, B.,
Lakshmi, C. S., ... & Raju, B. D. P. (2011),Green synthesis of silver
nanoparticles using Ocimum leaf extract and their characterization, Digest
Journal of Nanomaterials and Biostructures, 6(1), 181-186. (Silver nanoparticles
were synthesized from aqueous silver nitrate (1mM) through a simple and eco-
friendly route using leaf broth of Ocimum sanctum as reductant and stabilizer.
The aqueous silver ions when exposed to leaf broth were reduced and resulted in
the green synthesis of silver nanoparticles ranges from 3-20 nm.)
16. Park, Y., Hong, Y. N., Weyers, A., Kim, Y. S., & Linhardt, R. J.
(2011),Polysaccharides and phytochemicals: a natural reservoir for the
green synthesis of gold and silver nanoparticles,IET nanobiotechnology, 5(3),
69-78. (The various categories of compounds in plants that have potent biological
activities, phytochemicals are emerging as an important natural resource for the
synthesis of metallic nanoparticles. The focus of this review is the application of
polysaccharides and phytochemicals in the green synthesis of gold and silver
nanoparticles to afford biocomposites with novel uses in nanomedicine and as
nanocomposites.)
17. Kumar, K. P., Paul, W., & Sharma, C. P. (2011),Green synthesis of gold
nanoparticles with Zingiber officinale extract: characterization and blood
compatibility,Process Biochemistry, 46(10), 2007-2013.(The synthesized gold
nanoparticles,with a particle size ranging from 5 to 15 nm, using Zingiber
officinale extract which acts both as reducing and stabilizing agent. Z. officinale
extract is reported to be a more potent anti-platelet agent than aspirin. Therefore,
green synthesis of gold nanoparticles with Z. officinale extract, as an alternative
to chemical synthesis, is beneficial from its biological and medical applications
point of view, because of its good blood biocompatibility and physiological
stability.)
18. Ding, L., Zhou, P. J., Li, S. Q., Shi, G. Y., Zhong, T., & Wu, M.
(2011),Spectroscopic studies on the thermodynamics of L-cysteine capped
CdSe/CdS quantum dots—BSA interactions. Journal of fluorescence, 21(1),
17-24. Gel of tapioca starch (TS) is a suitable matrix for the formation of ZnS,
CdS and core-shell ZnS/CdS as well as CdS/ZnS quantum dots (QDs). These QDs
reside in the matrix as non-agglomerating 3 - 10 nm nanocrystals. It is
demonstrated that amylopectin is responsible for the QDs formation rather than

7
amylose. Combination of ZnS with CdS in the core-shell QDs results in the
increase in the intensity of emission without any shift of its wavelength.
19. Yang, T. T., Chen, W. T., Hsu, Y. J., Wei, K. H., Lin, T. Y., & Lin, T. W.
(2010). Interfacial charge carrier dynamics in core− shell Au-CdS
nanocrystals, The Journal of Physical Chemistry C, 114(26), 11414-11420. (Au-
CdS nanocrystals can be used as highly efficient photocatalysts which may
practically harvest energy from sunlight.)
20. Engelbrekt, C., Sørensen, K. H., Zhang, J., Welinder, A. C., Jensen, P. S., &
Ulstrup, J. (2009),Green synthesis of gold nanoparticles with starch–glucose
and application in bioelectrochemistry, Journal of materials Chemistry,
19(42), 7839-7847.(Gold nanoparticle (AuNP) synthesis from buffered glucose
and starch solution has been developed and the particles investigated by UV-Vis
spectroscopy, transmission electron microscopy(TEM), atomic force microscopy
(AFM) and electrochemistry. The synthesis proceeds smoothly in neutral and
basic solution. The starch concentration, temperature and chemical nature of the
buffers are key factors in the AuNP formation. Glucose and starch are reducing
and protecting agents,respectively. Among several inorganic and biological
Good’s buffers, phosphate and MES buffers give the best results with quite
uniform AuNPs.)
21. Kemp, M. M., Kumar, A., Mousa, S., Park, T. J., Ajayan, P., Kubotera &
Linhardt, R. J. (2009),Synthesis of gold and silver nanoparticles stabilized
with glycosaminoglycans having distinctive biological activities,
Biomacromolecules, 10(3), 589-595.(These nanoparticles were prepared by
reducing AuCl4 and AgNO3 using heparin and hyaluronan as both reducing and
stabilizing agents. The particles show stability under physiological conditions and
narrow size distributions for heparin particles and wider distribution for
hyaluronan particles. Studies show that the heparin nanoparticles exhibit
anticoagulant properties.)
22. Chen, W. T., Yang, T. T., & Hsu, Y. J. (2008),Au-CdS core− shell
nanocrystals with controllable shell thickness and photoinduced charge
separation property, Chemistry of Materials, 20(23), 7204-7206.(A facile and
reproducible approach for preparing Au-CdS core-shell nanocrystals with
controllable shell thickness. The photoinduced charge separation property was
demonstrated and revealed in the as-synthesized Au-CdS nanocrystals. The
present synthetic route can be readily extended to obtain other sulphide
semiconductor-coated Au nanocrystals such as Au-ZnS.)

8
23. Rodriguez, P., Munoz-Aguirre, N., Martínez, E. S. M., Gonzalez, G., Zelaya,
O., & Mendoza, J. (2008), Formation of CdS nanoparticles using starch as
capping agent, Applied surface science, 255(3), 740-742.(CdS nanoparticles
have been synthesized using starch as capping agent in aqueous solution. The
morphology and crystalline structure of such samples were measured by high-
resolution transmission electron microscopy and X-ray diffraction, respectively.
The average grain size of the nanoparticles determined by these techniques was
of the order of 5 nm. Photoluminescence of CdS nanoparticles shows a strong
emission peak below to the band gap bulk semiconductor.)
24. Chandran, S. P., Chaudhary, M., Pasricha, R., Ahmad, A., & Sastry, M.
(2006), Synthesis of gold nanotriangles and silver nanoparticles using
Aloevera plant extract, Biotechnology progress, 22(2), 577-583.(The kinetics
of gold nanotriangle formation was followed by UV-vis-NIR absorption
spectroscopy and transmission electron microscopy (TEM). The effect of
reducing agent concentration in the reaction mixture on the yield and size of the
gold nanotriangles was studied using transmission electron microscopy.
Monitoring the formation of gold nanotriangles as a function of time using TEM
reveals that multiply twinned particles (MTPs) play an important role in the
formation of gold nanotriangles.)
25. Huang, H., & Yang, X. (2004), Synthesis of polysaccharide-stabilized gold
and silver nanoparticles: a green method, Carbohydrate research, 339(15),
2627-2631.(A simple, green method was developed for the synthesis of gold and
silver nanoparticles by using polysaccharides as reducing/stabilizing agents. The
obtained positively charged chitosan-stabilized gold nanoparticles and negatively
charged heparin-stabilized silver nanoparticles were characterized with UV-vis
spectroscopy and transmission electron microscopy.)
26. Talapin, D. V., Koeppe, R., Götzinger, S., Kornowski, A., Lupton, J. M.,
Rogach & Weller, H. (2003). Highly emissive colloidal CdSe/CdS
heterostructures of mixed dimensionality, Nano Letters, 3(12), 1677-1681.
(The efficient shape control may be achieved in the shell of colloidally grown
semiconductor nanocrystals (independent of the core), allowing the combination
of a 0-D spherical CdSe core with a 1-D rodlike CdS shell.)

9
3. MATERIALS AND METHODS
3.1 MATERIALS USED:
 Gold Chloride.(AuCl)
Auric chloride, is a chemical compound of gold and chlorine. With the
molecular formula Au2Cl6.Gold (III) chloride is very hygroscopic and
highly soluble in water as well as ethanol. It decomposes above 160 °C or
in light.
 Reducing agent (Tulsi and Pomegranate Extract).
 Cadmium Acetate.
Cadmium acetate is the chemical compound with the formula
Cd(CH3CO2)2. This colourless solid is classified coordination polymer,
featuring acetate ligands interconnecting cadmium centers. The compound
exists in anhydrous form and as a dihydrate. It forms by treating cadmium
oxide with acetic acid:
CdO + 2 CH3COOH → Cd(CH3COO)2 + H2O

Figure 3.1 – Structure of Cadmium acetate

 L-Cysteine.
Cysteine is a semiessential proteinogenic amino acid with the formula
HO2CCH(NH2)CH2SH. The thiol side chain in cysteine often participates
in enzymatic reactions, as a nucleophile. The thiol is susceptible to
oxidation to give the disulfide derivative cystine, which serves an
important structural role in many proteins.

Figure 3.2 – Structure of L-cysteine

10
 DDT
Dichlorodiphenyltrichloroethane, commonly known as DDT, is a
colorless, tasteless, and almost odorless crystalline chemical compound, an
organochlorine. Originally developed as an insecticide, it became infamous
for its environmental impacts.
Human health effects from DDT at low environmental doses are unknown.
Following exposure to high doses, human symptoms can include vomiting,
tremors or shakiness, and seizures. Laboratory animal studies showed
effects on the liver and reproduction. DDT is considered a possible human
carcinogen.

Figure 3.3 – Structure of DDT

 RHODAMINE B
Rhodamine B is a chemical compound and a dye. It is often used as
a tracer dye within water to determine the rate and direction of flow and
transport. Rhodamine dyes fluoresce and can thus be detected easily and
inexpensively with fluorometers.
The acute exposure to Rhodamine B leads to burning of the eyes (82%),
excessive tearing, nasal burning, nasal itching, chest pain, rhinorhea,
cough, dyspnea, burning of the throat, burning/pruritic skin, chest
burning, headache and nausea.

11
3.2 METHODOLOGY:
I. SYNTHESIS OF GOLD NANO PARTICLES
Gold Nanoparticles are synthesised from extracts of Tulsi (Ocimum sanctum) and
Pomogranate (Punica granatum).
II. SYNTHESIS OF CdS QUANTUM DOTS
CdS Quantum Dots are prepared by using Cadmium acetate and L-cysteine by
using Hydrothermal Method.
III. SYNTHESIS OF Au-CdS QUANTUM DOTS
Au-CdS Quantum Dots are synthesised by using L-cysteine. The hydrothermal
Reaction taking place at 130ºC decomposes cysteine to Au-CdS Quantum Dots.
3.2.1 SYNTHESIS OF GOLD NANOPARTICLES: BY TULSI LEAF
• 100 g of Tulsi (Ocimum sanctum) are washed with Distilled water. Then
mixture is boiled for about one hour at 74ºC and it is Centrifuged at 3500
rpm for 15 minutes. Filtered by using Whatman filter paper No.41 .
• 0.002 g ( 1 mM) of Gold Chloride Solution is prepared in 10 ml Deionised
water and 30 ml leaf Extract was added.
• Stirred in Magnetic stirrer at 800 rpm for 24 hours at Room Temperature
(36ºC) and sonicated for 8 cycles.
• Then the Sample was dried by using Hot air oven at temperature of 70ºC
for 12 hours.

Figure 3.4 – Leaf Extract of Ocimum sanctum (Tulsi)

12
 3.2.2 SYNTHESIS OF GOLD NANOPARTICLES: BY
POMEGRANATE PEELS
• 7.5 g of Pomegranate (Punica granatum) powdered peels are taken and
dissolved in 100 ml of Deionised Water.
• Stirred in magnetic stirrer at 800 rpm for 24 hours .
• Filtered by using Whatmann filter paper no.41 and clear solution is
obtained.
• 0.002 g ( 1 mM) of Gold Chloride Solution is prepared in 10 ml Deionised
water and 30 ml Extract was added.
• Stirred in Magnetic stirrer at 800 rpm for 24 hours at Room Temperature
(36ºC) and sonicated for 8 cycles.
• Then the Sample was dried by using Hot air oven at temperature of 70ºC
for 12 hours

Figure 3.5 - Pomegranate Extract Stirred in magnetic stirrer

13
Figure 3.6 - Gold nanoparticles by pomegranate and tulsi extract

14
3.2.3. Synthesis of Cadmium Sulphide Quantum Dots by Hydrothermal
Method
Hydrothermal synthesis includes the various techniques of crystallizing
substances from high-temperature aqueous solutions at high vapor pressures.
Aqueous solution of L-cysteine was mixed with cadmium acetate in 2:1 molar
ratio of cysteine to cadmium in 30 ml of deionised water. The reaction is carried
out in a steel pressure vessel called autoclave .It is transferred to Teflon lined
autoclave (50ml capacity) that was sealed and hydrothermal reaction is carried
out at 130° C for 6 hours.
Then the sample was centrifuged and washed with water to remove impurities.

Figure 3.7 – Reactants in Teflon rod

Figure 3.8- Autoclave Reaction vessel

15
3.3 DEGRADATION OF DDT BY GOLD NANOPARTICLES

I. Preparation of DDT Stock Solution

The DDT Stock solution is prepared by dissolving 1ml of DDT solution (16.7%
) in 100ml of Water-Acetone Mixture in 9:1 Ratio.
II. DDT Degradation by using Gold Nanoparticles
1 mg of gold nanoparticles is dissolved in 100 ml of DDT stock solution and
degradation is carried out in magnetic stirrer and 5 ml of sample is withdrawn
for different interval for 1h,2h,3h,4h,5h,24h and 48h.

Figure 3.9 – DDT Stock Solution

Figure 3.10 – Samples after Degradation

16
 DEGRADATION OF RHODAMINE B DYE BY PHOTOCATALYTIC
REACTION
• The 10 ppm Rhodamine B Dye solution is prepared by dissolving 0.025 g
in 250 ml of water.
• The 100 ml of Rhodamine B is feed to Photocatalytic Reactor and 10 mg
of Cadmium Sulphide Quantum Dots is added.
• It is stirred in darkness for about 30 minutes.
• The Photocatalytic Reaction is carried out in Photocatalytic Reactor and
sample is withdrawn in time interval of 40 minutes.

Figure 3.11 – Rhodamine Dye solution and Degradation of Rhodamine B in

Photocatalytic Reactor.

Figure 3.12 - Schematic diagram of photo chemical reaction

17
4. RESULTS AND DISCUSSION:
4.1. GOLD NANOPARTICLES SAMPLE 1 AND 2:
4.1.1 UV ANALYSIS:
UV–vis spectroscopy is an important technique to ascertain the formation and
stability of metal nanoparticles in aqueous solution. Colour of gold colloid is
attributed to surface plasmon resonance. The UV-Vis spectra shows the Surface
plasmon Resonance occurs at 542 and 550 nm for gold nanoparticle sample 1 and
sample 2 respectively.

Figure 4.1 - UV Analysis for gold nanoparticle sample 1

‘

18
 Figure 4.2 - UV Analysis for gold nanoparticle sample 2
4.1.2 FTIR ANALYSIS:
FTIR measurements were carried out to identify the functional groups in Au (I)
and (II) responsible for capping leading to the efficient stabilization of the gold.
The FTIR analysis used to identify possible biomolecules present in extracts of
Ocimum sanctum and Punica granatum Extracts. The IR spectrum of gold
nanoparticles manifests prominent absorption bands located at 1017, 1229, 1511
and 1630, 1860 cm-3.

19
 Figure 4.3 - FTIR Analysis of Gold nanoparticles 1 and 2
4.1.3 XRD ANALYSIS

The crystalline nature of Gold nanoparticles was further confirmed from X-ray
diffraction (XRD) analysis. The XRD pattern of the dried nanoparticles obtained
from gold colloid. Five diffraction peaks are observed in the reflections in the
structure of metallic gold, respectively (JCPDS no. 04-0784), revealing the
Synthesised nanoparticles are crystalline gold nanoparticles.

20
Figure 4.4 – XRD Analysis of Gold Nanoparticles 1 and 2.

21
 Pos. [°2θ] Height FWHM d- D(nm)
[cts] spacing
[Å]
15.43 60.05 0.2558 5.74 31.36
17.29 139.09 0.2047 5.12 39.29
24.33 165.57 0.4605 3.65 17.66
25.67 147.49 0.3070 3.46 26.56
27.88 325.72 0.1535 3.19 53.37
29.79 160.02 0.4093 2.99 20.10
31.38 268.51 0.2047 2.85 40.34
32.10 1114.37 0.0624 2.78 132.58
32.21 2137.78 0.0384 2.77 215.50
34.09 184.56 0.1535 2.62 54.17
38.78 1342.81 0.1279 2.32 65.89
40.01 262.93 0.1791 2.25 47.24
44.91 514.86 0.1535 2.01 56.04
47.20 115.12 0.3744 1.92 23.17
48.89 141.47 0.1092 1.86 79.97
52.39 55.71 0.3744 1.74 23.66
54.33 61.76 0.3744 1.68 23.86
55.99 52.15 0.0624 1.64 144.30
56.91 634.59 0.0624 1.61 144.91
57.05 370.66 0.0624 1.61 145.01
65.03 327.50 0.4992 1.43 18.88
66.65 298.07 0.0936 1.40 101.65
66.85 176.12 0.0936 1.40 101.77
75.64 638.90 0.0780 1.25 129.03
75.85 346.41 0.1248 1.25 80.76
78.25 337.52 0.3120 1.22 32.84
82.28 121.53 0.6240 1.17 16.91
84.34 285.43 0.1560 1.14 68.76

TABLE 4.1 - XRD CALCULATION (GOLD NANOPARTICLES SAMPLE 1)

22
 Pos. Height FWHM d-spacing D(nm)
[°2θ] [cts] Left [Å]
[°2θ]
9.5671 107.72 0.6140 9.24476
12.99
12.1801 139.19 0.1535 7.26674 52.09
18.0613 325.05 0.1279 4.91160 62.94
24.7719 500.61 0.1535 3.59418 53.03
27.0539 454.25 0.3070 3.29598 26.64
27.8927 903.33 0.1535 3.19873 53.37
38.1142 3385.20 0.2814 2.36114 29.89
44.1459 1134.01 0.1872 2.04983 45.83
44.2996 1168.39 0.0936 2.04815 91.71
52.1557 39.12 0.4368 1.75230 20.26
64.6477 569.38 0.3120 1.44061 30.15477
77.4896 754.63 0.4992 1.23080 20.41978
81.4911 237.53 0.3744 1.18017 28.02869

TABLE 4.2 - XRD CALCULATION (GOLD NANOPARTICLES SAMPLE 2)

23
4.1.4 SEM ANALYSIS
A scanning electron microscope (SEM) is a type of electron microscope that
produces images of a sample by scanning the surface with a focused beam
of electrons. The SEM gives morphology of gold nanoparticles.

Figure 4.5 - SEM Analysis of gold sample 1

Figure 4.6 - SEM Analysis of gold sample 2

24
4.1.5 EDAX ANALYSIS:

I. GOLD NANOPARTICLES SAMPLE 1:

ELEMENT ATOMIC WT(%) ATOM(%)

NUMBER

C 6 61.37 71.09
O 8 29.59 25.74
Au 79 2.45 0.17
Na 11 1.90 1.15
K 19 1.88 0.67
Cl 17 0.83 0.72

Mg 12 0.53 0.30

Cl 20 0.45 0.16

TABLE 4.3 – EDAX TABLE FOR GOLD NANOPARTICLE I

Figure 4.7 - EDAX ANALYSIS FOR GOLD NANOPARTICLE I

25
II. GOLD NANOPARTICLES SAMPLE 2:

ELEMENT ATOMIC WT(%) ATOM(%)

NUMBER

C 6 59.13 69.93
O 8 30.28 26.88
Au 79 3.85 1.40
Na 11 3.41 0.25
K 19 2.25 0.90
Cl 17 0.69 0.43

Mg 12 0.25 0.15

Cl 20 0.15 0.06

TABLE 4.4 – EDAX TABLE FOR GOLD NANOPARTICLE II

Figure 4.8 - EDAX ANALYSIS FOR GOLD NANOPARTICLE II

26
4.1.6 RAMAN SPECTROSCOPY:
I. GOLD NANOPARTICLES SAMPLE 1:

Figure 4.9 –
RAMAN SPECTROSCOPY ANALYSIS FOR GOLD NANOPAARTICLES I
POSITION ( cm-1 ) FUNCTIONAL GROUP
1154 Aromatic Ring
1416 CH3, CH2 Deformation
2702 SH
3010 CH
3394 OH
3550 OH

TABLE 4.5 – RAMAN ANALYSIS FOR GOLD NANOPARTICLES I

27
II. GOLD NANOPARTICLES SAMPLE 2 :

Figure 4.10 –
RAMAN SPECTROSCOPY ANALYSIS FOR GOLD NANOPAARTICLES II

POSITION ( cm-1 ) FUNCTIONAL GROUP

1450 CH3, CH2 Deformation
2264 C=C
3026 OLEFINIC CH
3172 OH
3382 OH
3552 OH

TABLE 4.6 – RAMAN ANALYSIS FOR GOLD

NANOPARTICLES II

28
4.2. CADMIUM SULPHIDE QUANTUM DOTS:
4.2.1 UV ANALYSIS:
Optical properties of synthesized water dispersible QDs were characterized by
UV-Vis spectrometry. The maximum absorbance was at 412 nm.

Figure 4.11 – UV Analysis of Cadmium Sulphide Quantum Dots

29
 Figure 4.12 - Photographs of Cadmium sulphide Quantum dots under Visible
length and Ultra violet light

30
4.2.2 FTIR ANALYSIS

Figure 4.13 - FTIR Analysis of Cadmium Sulphide Quantum Dots

Frequency cm-1 Functional Group

548,648 Halogen compounds

1041 C-O Bond

1297 Amide

1393 CH3 Bend

1597 Aromatic

TABLE 4.7 – FTIR ANALYSIS OF CADMIUM SULPHIDE

31
4.2.3 XRD ANALYSIS:
The XRD Analysis was carried out with Cu Kα (1.54 Ã) Radiation. The XRD
peaks values are found to be 11.96°,23.93°,36.19° corresponding to (111), (220),
(311) planes respectively. This is in agreement with JCPDS data (no. 10-454). A
considerable broadening of diffraction peaks is the characteristic feature of the x-
ray diffraction pattern films of cadmium sulphide. This broadening of the
diffraction peaks is associated with the small sizes of particles in domains in
films.

Figure 4.14- XRD Analysis of Cadmium Sulphide Quantum dots

32
4.2.4 SEM ANALYSIS:
The Morphology of Cadmium Sulphide Quantum dots are studied by using SEM
Analysis.

Figure 4.15 – SEM ANALYSIS OF CdS

33
4.2.5 RAMAN SPECTROSCOPY:

Figure 4.16 - RAMAN SPECTROSCOPY ANALYSIS FOR CADMIUM

SULPHIDE

POSITION ( cm-1 ) FUNCTIONAL GROUP

1172 C-C
2316 C≡C
3386 OH
3540 OH

TABLE 4.7 – RAMAN ANALYSIS FOR CADMIUM

SULPHIDE

34
4.3 DDT DEGRADATION ANALYSIS BY USING GOLD
NANOPARTICLE SAMPLE 1 AND 2:
The absorbance of the supernatant was measured using a UV-Vis
spectrophotometer at various wavelengths. The degradation of DDT was
estimated according to the following equation

Degradation (%) = (1−At/A0) × 100

Where A0 is the initial absorbance and At is the absorbance after time t at the
wavelength corresponding to the peak maximum.
The initial Absorbance values of sample 1 and 2 are 0.82 and 1.98.

Figure 4.16 – DDT Degradation studies by gold nanoparticle sample 1

35
 Time Absorbanc Degradati
(h) e (a.u) on (%)
1 0.74 9.756

2 0.67 18.292
3 0.6 26.829
4 0.54 34.146
5 0.49 40.243
24 0.43 47.560
48 0.4 51.219

Table 4.5 – DDT Degradation studies by gold nanoparticle sample 1

Figure 4.17- DDT Degradation studies by gold nanoparticle sample 2

36
 Time Absorbance Degradation
(h) (a.u) (%)
1 1.51 23.737
2 1.22 38.383
3 0.91 54.040
4 0.75 62.121
24 0.64 67.676
48 0.58 70.707

Table 4.6 - DDT Degradation studies by gold nanoparticle sample 2

37
4.4 DEGRADATION OF RHODAMINE B USING CADMIUM
SULPHIDE QUANTUM DOTS AS PHOTOCATALYST:

Figure 4.18 - DDT Degradation studies by Cadmium sulphide

TIME(Minutes) ABSORBANCE DEGRADATION(%)

40 1.46 17.04545
80 1.37 22.15909
120 1.34 23.86364
160 1.27 27.84091
200 1.18 32.95455
240 1.104 37.27273

Table 4.7 – Degradation studies by Cadmium sulphide

38
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