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Experiment 8: Synthesis of Gold and Silver Nanoparticles

Abstract

To better understand the colloidal properties of nanoparticles, synthesis of gold

and silver nanoparticles was attempted. Synthesis of nanoparticles was confirmed

with qualitative color changes after citrate reduction. The Tyndall effect was

observed in both colloidal solutions. The absorption peaks (SPR) were obtained in

the visible range, with max of approximately 610 and 300 nm for gold and silver,

respectively. Filtration did not yield any particles greater than 20 nm.

Introduction

Nanoparticles are particles ranging typically from 1 to 100 nanometers. Nanoparticles

have applications in a wide variety of fields, including removing environmental contaminants

such as DDT. Gold and silver nanoparticles are of interest given the potential for high scale

production and their relative stability to other metal nanoparticles.

Colloids are typically composed of nanoparticles suspended in a solvent. Colloids, such

as fog or smog, are of interest given their ability to demonstrate the Tyndall effect, or light

scattering of particles, as opposed to a non-colloidal solution in which light simply passes

through without scattering. As it pertains to this experiment, gold and silver nanoparticles can

exhibit the Tyndall effect, which can be observed to determine nanoparticle size.

Gold and silver nanoparticles can be synthesized in a variety of ways, but most involve

reducing agents to reduce gold and silver. The reducing agents are also of significance. The
Brust process, for example, involves using the highly volatile NaBH4 (sodium borohydride)

which is limited due to its thiol incompatibilities and hazardous synthesis process despite being a

relatively reliable technique.1 In contrast, using sodium citrate as a reducing agent is a safer and

simpler alternative.

Through the Turkevich method, sodium citrate can be used to reduce gold and silver.

After reducing agents are added to heated gold and silver precursors, changes in color can

indicate existence of nanoparticles through the colloidal property. Additionally, observing UV-

vis peaks can specify properties of nanoparticles, such as size and shape.

Experimental

2 mL of 0.5 mM hydrogen tetrachloroaurate (III) trihydrate HAuCl4 3H2O solution was

placed in a test tube and set in a boiling water bath. 2 mL of 0.5 mM AgNO3 was placed in a test

tube and set to heat at 60 C. Both solutions were heated for 5 minutes, after which 5 drops of

1% sodium citrate was added to each test tube. Solutions were heated until color change became

evident (yellow for silver and red for gold). Solutions were removed from heat and allowed to

cool. A test tube was filled with distilled water, and a laser was shone through the water and each

solution. The tubes were poured into separate Petri dishes. Using a syringe, 1 mL of air was

drawn, as well as the silver mixture. A 20 nm pore size ceramic filter was attached. The plunger

was slowly depressed and the mixture and air were forced through the filter. The color of the

filtrate was observed. About 100 mg of NaCl was added to the gold solution. Another syringe

was used to draw 1 mL of air and the gold mixture. The plunger was again depressed and the

mixture and air were forced through the filter. The color of the filtrate was observed. Finally,
each filter was cut open and the color inside the filter was observed. Ultraviolet-visible

spectrophotometer was used to measure absorbance vs wavelength of each nanoparticle solution.

Data and Observations

Figure 1. UV-Vis spectrum of AgNPs colloidal solution

Figure 2. UV-Vis spectrum of AuNPs colloidal solution


Results and Discussion

Gold and silver nanoparticles were synthesized through citrate reduction, as indicated by

color changes in solution. Gold nanoparticles were indicated by red color in solution, and silver

nanoparticles were indicated by yellow color in solution. The Tyndall effect was observed by

shining a laser through a test tubes of water and each nanoparticle solution.

Unfortunately, analysis of UV-Vis spectra indicates no broad peaks that would be

expected otherwise from complete synthesis of gold and silver nanoparticles. There are no

discernable peaks in the spectra for the silver nanoparticle, and a single very broad peak in the

spectra for the gold nanoparticle. For the silver nanoparticle, it is likely accuracy was affected

due to taking the UV-Vis after beginning the filtration step. Air drawn by the syringe would

likely have affected the precision of the spectrophotometer. For future experiments, it is

advisable to perform UV-Vis prior to the filtration step.

Lambda max (max) was found to be 610 nm and 300 nm for gold and silver, respectively.

Ideally, lambda max (max) should be clearly represented with taller and more defined peaks

where molecules will absorb in a wavelength range. Generally, the higher the max, the smaller

the nanoparticles. For gold, the max should have been closer to 520 nm given the size dependent

physical properties of gold and the fact that the solution after adding sodium citrate became a

shade of red. Assuming the max obtained for gold is accurate, the color of the solution shouldve

been closer to purple-pink, which exhibits a higher max as well as larger nanoparticles (100 nm

vs 20 nm in red colored solution.

For the silver nanoparticle, max is difficult to pinpoint especially given the fact there is

no clearly defined peak and instead resembles an inverse logarithmic function, which is
problematic to analyze. This can be mostly attributed to human error and the faults listed above.

There should also be more clearly defined peaks in the UV-vis spectra for the silver. Assuming

nanoparticle size was greater than 20 nm, the size of the ceramic filters, nanoparticle size would

have been observed through filtration. Centrifugation would also have been another option to

filter nanoparticles.

Conclusion

Developing novel methods for characterizing and manipulating nanoparticles is at the

forefront of nanotechnology research today. Synthesis of gold and silver nanoparticles through

sodium citrate synthesis could be a prelude to larger scale production of nanoparticles. Although

the UV-vis spectra of both metallic colloids did not yield any clearly defined peaks, it can be

assumed that performing the spectroscopy step before the filtration step would have led to better

accuracy.

References

1. M. Brust, J. Fink, D. Bethell, D. J. Schiffrin, and C. Kiely, Synthesis and reactions of

functionalised gold nanoparticles, Journal of the Chemical Society, Chemical Communications,

no. 16, pp. 1655-1656, 1995.


Discussion Question:

1.) Au3+(aq) + 3 e-- >> Au (s)

2.) Physical properties of nanoparticles can vary with the size of nanoparticles. Gold

nanoparticles, for example, differently colored particles in solution will correspond to different

sized particles. Whereas purple colored solution indicates 100 nm nanoparticles, red colored

solution indicates smaller, 20 nm particles, and brown-yellow colored solution indicates the

smallest particles, at 1 nm.