Chemistry Extended Essay Proposal

Name Rebecca Kua Rui Xuan

Class 5.09

HL Subjects Literature, Chemistry, Biology

Chemistry Teacher Mr Tan Keng Hsin

Topic Biosynthesis of Iron Nanoparticles using plant

extracts

Research Question How does pH affect the rates of adsorption of

three common pollutants: Lead (II), Copper
(II) ions, and malathion insecticide in water
using Iron nanoparticles biosynthesized from
Camellia sinesis leaf extract?

1. Research Question:
How does pH affect the rate of adsorption of Lead (II), Copper (II) ions, and malathion
insecticide in water using Iron nanoparticles biosynthesized from Camellia sinesis leaf
extract?

2. Motivation Behind the Research

With the growing problem of environmental pollution and climate change, I was inspired
by the increasing focus on sustainability in scientific research to combat the impacts of
chemical pollutants on the natural environment. I have seen documentaries on various
types of industrial waste pollution that are affecting human health and aquatic life in
many countries currently, for example Lead pollutants found in drinking water can cause
neurological damage to humans. Hence I felt strongly about finding a way to mitigate the
harmful impacts of our actions on our planet, and ourselves.

I have researched on the different techniques to produce metallic nanoparticles, including

Iron oxide nanoparticles(γ-Fe2O3 NPs). Traditionally, metal or metal oxide NPs were
mostly synthesized through physical or chemical means such as microwave irradiation
and sol-gel method, which may often involve toxic reactants which can have a negative
impact on one’s health and the environment, and require expensive equipment and large
amounts of energy to produce them. However, plant polyphenols were found to have
reducing properties which led to safer, faster, eco-friendly and more cost-effective
methods of producing NPs that can be conducted at room temperature and pressure.
 In particular, I was fascinated by the wide variety of properties of nanoparticles
synthesized from green tea leaf extract (Camellia sinesis). Green tea is rich in polyphenol
antioxidants and other secondary metabolites: phenolic acid, alkaloids, flavonoids,
catechins and is able to reduce Fe(II) and (III) ions into bulk formation of iron
nanoparticles at room temperature. Plant extracts are renewable and naturally-derived
sources thus minimizing the environmental impacts during the synthesizing process. I
would like to find out the effect of pH on the rate of breaking down of heavy metal
pollutants and synthetic insecticides, and deduce the optimal pH needed to remove as
many contaminants in the water as possible.

3. Background information

3.1. Synthesis of nanoparticles

Nanoparticles are very small particles that have a diameter of anywhere between 1 to 2500 nm.
Due to their large surface area to volume ratio,high porosity and high solubility, nanoparticles
are highly reactive and have a wide variety of applicable uses, such as the absorption and
transport of medicinal compounds as well as catalyzing reactions. The biosynthesis of Iron NPs
involves a two step redox reaction using plant-based tea leaf extracts as the reducing agent(for
example: Camellia sinesis), in reducing iron (II) and (III) ions into either forms of iron
nanoparticle: maghemite(γ-Fe2O3) or magnetite(Fe3O4).

Fig. 1 The formation of iron nanoparticles, magnetite and maghemite, from reducing Fe2+ and
3+

The methods of nanoparticle synthesis can be generalized into two ways: Top-down and Bottom-
up approach. In the biosynthesis of Iron NPs, it is a bottom-up approach whereby individual
atoms and molecules react to form larger nanostructures. A Top-down approach involves the
decomposition of large materials into its constituent nanostructures, for instance the sol-gel
technique in various metal oxide NPs production.

The heated and filtered Green tea extract prepared can be added to 0.01M of ferric chloride
solution in a 1:1 stoichiometric proportion in a stoppered conical flask. The reaction occurs
rapidly turning the dark yellow green tea extract solution into a black solution.

The obtained solution is then centrifuged with the liquid portion poured out after to remove
impurities in the iron nanoparticles. The remaining black precipitate is kept under inert
conditions to prevent oxidation into γ-Fe2O3 .
The concentration of iron nanoparticles can be determined by placing 1 mm quartz cuvettes of
the iron NPs in deionised water and a blank, in a UV/Vis spectrophotometer. Using Beer-
Lambert's Law, A=log10(Io/I),the absorbance is proportional to the concentration of the NPs. In
this investigation, the unoxidized magnetite form of iron NPs will be used for the adsorption
reaction as a constant variable. Different forms of nanoparticles differ in shape and reactivity,
thereby leading to inconsistent rate of reaction.

Fig.2: Two step reduction of Iron salt and oxidation of plant polyphenols

Fig. 3: Green tea leaf extract and solution formed on adding ferric chloride(aq)
(referenced from green-synthesis-of-iron-nanoparticles-using-green-tea-leaves-extract-2155-
983X-1000153)

Existing SEM micrographs have revealed that the NPs formed had a diameter of about 116nm, a
relatively small particle size which correlates with a higher reactivity.

3.2. Biosorption of 3 types of pollutants using green-synthesized nanoparticles

Lead and copper are examples of common heavy metals found in industrial waste, with ceramics
and acid-battery industries being the main contributors. Water-soluble compounds such as
Pb(NO3)2 and Cu(NO3)2 release Pb2+ and Cu2+ ions in water respectively. Heavy metals are
known to be bioaccumulative in animals and are ecotoxic, causing adverse health effects if
ingested in large amounts. One example of the remediation efforts of heavy metal ions is
Biosorption. The absorbate (pollutant) is separated from the water sample by concentrating at the
nanoscale-surface of the solid absorbent. The Iron oxide NPs have a high porosity and large
surface area, making them effective absorbents. The adsorption kinetics is dependent on
temperature, pH, initial concentration of absorbate and absorbent. In this research, buffer
solutions are used to study the effects of specific pH ranges on the rate of adsorption of the 3
pollutants in focus.

Malathion (C10H19O6PS2) is a type of organophosphate insecticide often used in agricultural

industries to control mosquito and other pest populations. In some animal species it can get
broken down into malaoxon, a more toxic compound, inhibiting the action of the enzyme
acetylcholinesterase essential in nerve impulses. Malathion is a yellowish-brown liquid with a
higher density than water, with a solubility of about 145 mg/L. Along with other organic
insecticides, it can contaminate soil and water bodies as surface run-off.

Fig. 4: Structure of malathion

 4. Approach, materials and Apparatus required
4.1 Materials used
Materials Quantity of materials

Commercial Green Tea 20 to 50g

Leaves (Japanese green tea
brand)

Ferric Chloride Anhydrous 200g

Deionised water 2000cm3

0.1M Lead(II) Nitrate 500cm3

solution

Copper (II) Nitrate (aq) 500cm3

84.3% Malathion 200cm3

insecticide solution

Potassium chloride 10g

Dilute Hydrochloric acid 200cm3

Copper sulfate 1 to 2g

Ammonium acetate 10g

Ethanoic acid 200cm3

0.2M Sodium hydroxide 500cm3

Potassium dihydrogen 300cm3

phosphate

Ammonium chloride 6g

Aqueous ammonia 50cm3

4.2 Apparatus
Apparatus Number of apparatus
Weighing balance 1

UV spectrophotometer 1

Centrifuge 1

Bunsen burner 1

Thermometer 1

1000cm3 measuring cylinder 1

Filter funnel 1

Test tube 5

1000cm3 Volumetric flask 1

4.3 Procedure
Part A- Synthesizing the nanoparticles
1. Weigh about 20g of green tea leaves on a weighing scale.
2. Measure 1000 cm3 of deionized water in a 1000 cm3 l measuring cylinder. Transfer the
water and leaves to a water bath.
3. Heat the mixture to 80 degrees celsius to obtain the leaves extract. Filter the extract from
the solution using a filter funnel.
4. Dissolve 1.622g of anhydrous ferric chloride in 1000 cm3 of deionised water and mix
thoroughly.
5. Measure the mass of green tea extract. Add the 0.01M ferric chloride to the extract in a
1:1 proportion in a conical flask.
6. Centrifuge the obtained solution to remove impurities. Pour out the liquid portion and
rinse the residue with deionised water.
7. Keep the iron pellets in a stoppered test tube for future use.

Part B- Preparing 5 Buffer solutions ranging from pH 2.0-10.0

 1. Prepare the buffer solution of pH 2 by dissolving 6.57g of KCl in water and add 119 cm3
of 0.1M HCl. Dilute to 1000cm3 in a volumetric flask.
2. Prepare the buffer solution of pH 4 by dissolving 0.25g of CuSO4 and 4.5g of ammonium
acetate in dilute CH3COOH and dilute to 100cm3 in a volumetric flask.

3. Prepare the buffer solution of pH 6 by adding 250cm3 of 0.2 M potassium dihydrogen

phosphate to 28.5 cm3 of 0.2 M NaOH and dilute to 1000cm3 in a volumetric flask.
4. Prepare the buffer solution of pH 8 by adding 50cm3 of 0.2 M potassium dihydrogen
phosphate to 46.8 ml of 0.2 M NaOH, dilute to 200cm3 in a volumetric flask.
5. Prepare the buffer solution of pH 10 by dissolving 5.4g of NH4Cl in 20cm3 of water and
add to 35cm3 of aqueous ammonia dissolved in 100cm3 water.

Part C- Rate of adsorption of pollutants

1. Add 20cm3 of Lead (II) Nitrate into 50cm3 of the pH 2 buffer and add the iron
nanoparticles in excess.
2. Using the UV-Vis spectrophotometer, the rate of decrease in concentration of Pb2+ ions
can be determined graphically against time.
3. Save the data from the spectrophotometer in a usb drive
4. Repeat the above steps 1-3 for the remaining buffer solutions
5. Repeat the above steps for Copper (II) Nitrate and Malathion.
6. Compare the trends in the graphs for different pHs across the 3 pollutants and conclude
the optimal pH for the fastest rate of adsorption.

5. Risk assessment
A) Chemical hazards
Chemical Nature of Storage Handling Disposal MSDS
used or hazard procedure procedure procedure reference
synthesized

Malathion Acute oral Store in bottle Conduct Dispose 91481

toxicity and tightly closed experiments properly and
skin and dry in a fume clean up any
sensitization hood spills

Aqueous Skin irritation Store in bottle Wear gloves Dispose 318604

ammonia and serious tightly closed and safety properly and
eye damage goggles when clean up any
handling spills

Iron (III) Corrosive, Store in Wear gloves Dispose to an 157740

chloride skin and eye original bottle and safety approved
irritation tightly closed goggles when waste bin
handling

Lead (II) Harmful if Store away Wear gloves Dispose 228621

Nitrate swallowed or from heat and safety properly and
inhaled, goggles, clean up any
causes conduct spills
allergic skin experiments
reaction and in a fume
eye damage hood

B) Non chemical hazards

Name of Purpose of Nature of Handling Reference

equipment equipment hazard procedure

Bunsen burner Heat mixture in Fire risk, burn Be careful of the Sigmaaldrich
preparation of hazard hot flame MSDS-bunsen
nanoparticles burner
References
https://www.intechopen.com/chapters/71103
https://pubs.rsc.org/en/content/articlelanding/2009/jm/b909148c
https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4908060/
https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5245755/
http://recentscientific.com/green-synthesis-iron-nanoparticles-used-green-tea-leaves
https://www.unep.org/cep/heavy-metals
https://link.springer.com/article/10.1007/s42452-019-1699-2#Abs1
https://www.hindawi.com/journals/ast/2022/7384924/
https://pubchem.ncbi.nlm.nih.gov/compound/Malathion
https://www.semanticscholar.org/paper/Green-Synthesis-of-Iron-Nanoparticles-Using-Green-
Ksv/e5007321a52d3a6fffcbd705c17bdda0aa16b3b0