Name : Suleman Qaiser

19100156

Synthesis And Characterization

of
Gold Nanoparticle
Introduction:
Nanoparticles are particles between 1 and 100 nanometers in size. Nanoparticle
is defined as a small object that behaves as a whole unit with respect to its transport and
properties. Particles are further classified according to diameter.Nanoparticles are a
bridge between bulk materials and atomic or molecular structures. A bulk material should
have constant physical properties regardless of its size, but at the nano-scale size-
dependent properties are often observed. Thus, the properties of materials change as their
size approaches the nanoscale and as the percentage of atoms at the surface of a material
becomes significant. For bulk materials larger than one micrometer (or micron), the
percentage of atoms at the surface is insignificant in relation to the number of atoms in
the bulk of the material. The interesting and sometimes unexpected properties of
nanoparticles are therefore largely due to the large surface area of the material, which
dominates the contributions made by the small bulk of the material.
Gold is a nobel metal with a golden metallic cluster.But when its
size is reduced to nanoscale its colour changes .This property conferred by the
interaction of light with electrons on the gold nanoparticle surface. At a specific
wavelength (frequency) of light, collective oscillation of electrons on the gold
nanoparticle surface cause a phenomenon called surface plasmon resonance resulting
in strong extinction of light (absorption and scattering). The particular wavelength, or
frequency, of light where this occurs is strongly dependant on the gold nanoparticle size,
shape, surface and agglomeration state.At different size gold nanoparticles have different
colour like blue (`~80-100 nm) , purple(30-80 nm) , red(~3-30 nm) , brown(~1.5-3 nm)
and even yellowish (<1 nm).

CatalyticaL Activity :
 Au is usually viewed as an inert metal, but surprisingly Au nanoparticles less
than 3–5 nm in diameter are catalytically active for several chemical reactions.For
example it is used specially for the oxidation of CO .Gold particles also behave like a
semiconductors due to the separation of their conduction and valence band.

Chemical Reduction:
Chemical reduction of Au salt is the most convenient and fastest way for the
synthesis of Au NPs with better control over size,shape and surface chemistry.Hussain
acrylate -reduction method is commonly used for this purpose.Formation of Gold
nanoparticles is basically ia redox reaction.

Experiment:
In this experiment first we synthesize Au nanoparticles using citrate reduction
method. Then we determine the concentration of nanoparticles using spectroscopic
method and at last we use dynamic light scattering (DLS) techiques.

Chemicals:
Following reagents will be used in this experiment.
1. Gold (III) Chloride Trihydrate HAuCl4.3H2O (0.5 mM)
2. Trisodium citrate dihydrate (20 mM)
3. Sodium Chloride ,NaCl (1 mM)

Apparatus:
1. UV-Visible Spectrometer
2. Zetasizer Nano ZSP (DLS)
3.Condenser
4. Round bottom flask (100 mL)
5.Two Beakers
. 6.Magnetic stir bar
7.Two Glass vials
8. Hot plate and oil bath
9..Analytical balance

Safety:
Nanoparticles present possible dangers, both medically and environmentally.Most of
these are due to the high surface to volume ratio, which can make the particles very
reactive or catalytic. They are also able to pass through cell membranes in organisms, and
their interactions with biological systems are relatively unknown.

1. Trisodium citrate : Causes Irritation to skin.eyes,and respiratory tract.

2.HAuCl4.3H2O : Corrosive and hygroscopic. Causes eyes and skin burns upon contact. It
also causes gastrointestinal tract burns.
Procedure:
Synthesis of Au NPs :

Add 25 mL of 1 mM of HAuCl4 solution to a round bottom flask and heat till the start of
reflux (Reflux: the process of boiling a liquid so that any vapour is liquefied and returned
to the stock.). Add 5 mL of 20 mM sodium citrate tribasic dihydrate solution (pre-heated
at 60 °C) to the above solution under reflux.Allow the obtained mixture to stir and
continue reflux for 30 min.Stop the heating after 30 min and left it to stir to bring the
temperature down to the room temperature. Observe the change in the color of solution
after the addition of sodium citrate solution. Finally, it will result in the formation of ruby
red colored gold nanoparticles having a diameter of ~15 nm with a characteristic surface
plasmon resonance (SPR) band appearing at~520 nm in their UV visible absorption
spectrum.

Examining Stability of Au NPs:

Record the UV visible spectra of as-prepared Au NPs and of those after the addition of
NaCl using UV visible Spectrophotometer. You should get a characteristic SPR peak of as
prepared Au NPs, which contains a lot of information regarding the size, size distribution,
shape and the concentration of the Au NPs. Aggregated Au NPs after the addition of NaCl
will show broadening of the SPR band and the appearance of a shoulder/another
absorption band at higher wavelength.Monitor the hydrodynamic radius and surface
charge on Au NPs using Zetasizer nano ZSP before and after the addition of NaCl.The
morphology of the Au NPs can be determined using transmission electron microscope
(TEM) or scanning electron microscope (SEM) operating in STEM mode, which you are
not, required to do at this stage. We will, however share with you the TEM/SEM images
of selected samples of Au NPs.

Results:
Max Abortion (A1 ) at SPR-Peak = 2.653
Absorbance at 450 nm (A2) = 1.646
Ratio : A1/A2=2.653/1.646 = 1.61
Diameter from the table
d = 14 nm
Now, we find concentration by using following formula
Conc. =A2/El
Value of E from the table No. 2
E = 1.76 * 10-9
So,
Conc. = 1.646/1.76 * 10-9
Conc. = 9.35 * 10-9
Discussion:
A colloid is a solution that has particles ranging between 1 and 1000 nanometers in
diameter, yet are still able to remain evenly distributed throughout the solution. These are
also known as colloidal dispersions because the substances remain dispersed and do not
settle to the bottom of the container.In this experiment gold nanoparticles are produced in
the aqueous solution.The colloids are the suspension of Gold nanoparticles in the
solution, usually water.The colour of the liquid is intense red colour which indicates that
the nanoparticles are less than 100 nm.The nanoparticles are prepared by the redox
reaction and then dissolved in water and heated.After boiling reducing agent was added
in the solution.Reducing agent in this case is Sodium Citrate..This reagent reduce gold
and change oxidation state of gold from +3 to 0 (neutral atom).During this process the
stirrer in the solution keep on moving to ensure that all the particles that form are of
uniform sizes.Stabilizing Agent (Citrate Ion in this case ) is used to prevent from
aggregation.Citrate Ion sticks to the nanoparticle surface forming ligands.The repulsion
between the citrate ion prevents the nanoparticle from sticking together.The size of ligand
determines the overall size of the nanoparticle.As a result different nanoparticle have
different spacing between their particles thats why absorb different wavelength of light
and show different color at different wavelength.
Then NaCl is added to one of the vials to show that ligands are replaced by
chloride ion which form stronger bond than Au NPs making a bigger particle changing
light red to red.The intensity of the color increases.If Sugar was added instead NaCl no
change would occur because it is not strong enough to replace the citrate ligands of Au
NPs.
The change in energy as the wave passes through a layer is a constant of the material for a
given wavelength and is called its absorption coefficient.
It is evident from the graph of wavelength vs absorption for both the
vials.We observe that the vial with drops of NaCL tend to show higher absorption for the
wavelength longer than 550 nm which is the result of the particular aggregation which
cause a phenomenon called Surface plasmon Coupling. This Phenomenon changes the
maximum absorption of light to higher wavelength which result in the change of color of
solution.