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Procedia Engineering 148 (2016) 1396 – 1401

4th International Conference on Process Engineering and Advanced Materials

Parametric Study on Gold Nanoparticle Synthesis Using Aqueous Elaise

Guineensis (Oil palm) Leaf Extract: Effect of Precursor Concentration
Tausif Ahmada, Muhammad Irfana, Sekhar Bhattacharjeea,*
a
Universiti Teknologi PETRONAS, Chemical Engineering Department Bandar Seri Iskandar, 32610, Perak, Malaysia

Abstract

In this study, gold nanoparticles (AuNPs) were synthesized by using aqueous extract of Elaise guineensis (oil palm) leaves without addition of
any external stabilizing agent. Effects of precursor concentrations (0.51 mM- 4.055 mM) on SPR absorbance and AuNP particle size distribution
were investigated. The synthesis reaction was monitored by measuring time-variant SPR spectrum of the reaction medium with a UV-vis
spectrophotometer. Biosynthesized AuNPs were characterized using TEM, DLS, UV-vis and FTIR spectroscopy. TEM image analysis showed
formation of predominantly spherical gold nanoparticles with mean particle diameter of 27.89±14.59 nm were formed using 1.53 mM gold
concentration. DLS data showed that AuNPs with hydrodynamic diameter 55.22 ± 42.86 nm were formed, indicating formation of multilayer
coatings of biomolecules present in the leaf extract on nanoparticles. Spherical, triangular, pentagonal and hexagonal gold nanoparticles with
mean particle diameter 22.88 ±8.21nm were formed when higher gold (III) precursor concentrations (4.055 mM) were used. FTIR analysis
revealed that carboxylic and phenolic compounds present in leaf extract played dual roles as reducing and stabilizing agents during synthesis of
AuNPs.
© 2016 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
© 2016 The Authors. Published by Elsevier Ltd.
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-reviewunder
Peer-review under responsibility
responsibility of
of the
the organizing
organizing committee
committee of
of ICPEAM
ICPEAM 2016
2016.

Keywords: Elaise guineensis; gold nanoparticles; green synthesis

1. Introduction

Synthesis of gold nanoparticles (AuNPs) has received intense research interests due to their widespread applications in diverse
fields such as electronics, biotechnology and medicine [1]. Their large surface area and small size make them suitable for various
medical applications [2]. Gold nanoparticles (AuNPs) are usually synthesized through various physical and chemical methods,
which are expensive and use hazardous chemicals that make them unsuitable for medical applications [3]. Gold nanoparticles are
also synthesized by using different microorganisms and plant extracts [4]. Different plants extracts such as Aloe vera, Alfalfa, Neem,
Mangifera indica leaf have been successfully utilized as reducing and stabilizing agents in synthesis of gold nanoparticles [5-8].
Plant extracts are preferred for synthesis of gold nanoparticles due to their excellent biocompatibility [9]. Plant extracts contain
several phytochemicals, which simultaneously act as reducing and stabilizing agents during synthesis of AuNPs. These bio
compounds form multilayer coating on the surface of AuNPs and thus increase their long-term stability. The biomolecules also
enhance utilization potential of AuNPs for medical applications by imparting their inherent medicinal properties [10].
Oil palm plants are cultivated in different tropical areas such as Malaysia, Thailand, Africa and South Africa. Oil palm leaves
are abundantly released as waste products from oil palm industries. Aqueous and alcoholic extracts of oil palm leaves are rich
sources of polyphenols, antioxidants, flavonoids and catechins [11]. A study on effect of gold percurser concentrations on size and

* Corresponding author. Tel.: +605-368 7640; +fax: 605-368 6176.

E-mail address: sekhar.bhatta@petronas.com.my

1877-7058 © 2016 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of the organizing committee of ICPEAM 2016
doi:10.1016/j.proeng.2016.06.558
 Tausif Ahmad et al. / Procedia Engineering 148 (2016) 1396 – 1401 1397

shape of AuNPs synthesized using (Elaise guineensis) oil palm leaves extract has not been reported in literature to the best of
auther’s knowledge. Objective of this study is to report experimental data on the effects of varying precursor concentrations on
particle size distribution and morphology of AuNPs synthesized by using aqueous oil palm leaf extract. Identification of
biofunctional groups present in oil palm leaf extract which are accountable for reduction, and stabilization of AuNPs are also
reported in this article.

Nomenclature

AuNPs Gold Nanoparticles

TEM Transmission Electron Microscope

FTIR Fourier Transform Infrared Spectroscopy
DLS Dynamic Light Scattering
SPR Surface Plasmon Resonance

2. Experimental

2.1 Materials and methods

Gold (III) chloride trihydrate (HAuCl4. 3H2O), 99.99 % purity was purchased from Sigma-Aldrich, Malaysia. Stock solution of
choloroauric acid (12.69 mM) was prepared by dissolving 500 mg of gold (III) chloride trihydrate in 100 ml deionized water. This
stock solution was further diluted with deionized water to prepare gold solutions of required concentrations. Oil palm leaves were
brought from a local oil palm mill, Felcra Berhad Nasaruddin Oil Palm Mill in Perak, Malaysia.

2.2 Preparation of oil palm leaf extract

Oil palm leaves were washed three times with deionized water and dried under sunlight for one week. The dried leaves were
washed again with deionized water to remove dust particles from the surface of oil palm leaves. These leaves were then dried in
oven for 8 hr at 70 ͦ C. The dried leaves were grinded in an IKA grinder to fine powder (0.25 mm) and subsequently packed in an
airtight box for further use.
Aqueous leaf extract was prepared by heating 1.0 g leaf powder in 20 ml of distilled water at 70 ͦ C for 10 min. The resulting
slurry was filtered with a Whatman 40 filter paper. The filtrate was stored at 4 ͦ C for further use in experiments.

2.3 Synthesis of gold nanoparticles

Gold nanoparticles were synthesized by adding 2 ml of aqueous extract to 7 ml of 1.53 mM aqueous gold (III) solution under
ambient conditions. The reaction medium was stirred at 30 ͦ C and 500 rpm for 60 min. Formation of AuNPs was visually identified
by observing color change of the reaction medium from light yellow to light red. The synthesis reaction was also monitored by
UV-vis spectrophotometric (400 nm–700 nm) scanning of aliquot samples collected from the reaction medium.

2.4 Characterization

Absorption spectra and SPR wavelength for AuNPs were recorded by using Perkin Elmer UV-vis spectrophotometer in 400 nm
to 700 nm range. Particle size distribution, mean particle diameter and morphology were studied with DLS (Malvern Zetasizer
Nano ZSP) and TEM (LIBRA 200FE). Identification of functional groups present in leaf extract and reaction medium was
performed with an FTIR Perkin Elma Spectrum (450 cm-1 to 4500 cm-1) spectrophotometer.

2.5 Effect of gold (III) concentration on synthesis of gold nanoparticles

Effect of gold (III) precursor concentration (0.51mM to 4.055mM) on size and shape of gold nanoparticles was evaluated by
carrying out AuNPs synthesis experiments at 30 ͦ C for 60 min. Absorption spectra were recorded after 60 min of reaction.

2.6Effect of volume of gold solution on synthesis of gold nanoparticles

1398 Tausif Ahmad et al. / Procedia Engineering 148 (2016) 1396 – 1401

Effect of volume of gold solution added to a fixed volume of aqueous leaf extract on synthesis of gold nanoparticles was studied
by changing volume of 1.53 mM gold (III) solution from 1ml to 5 ml. Volume of aqueous extract was kept constant at 2 ml in this
study.
2.6 Results and Discussions

The reaction medium changed its color from light yellow to light red after 8 min of stirring. Change in color of reaction medium
indicated formation of gold nanoparticles due to surface plasmon resonance (SPR) phenomenon [12]. The redox reaction involves
reduction of gold (III) ions to gold atoms primarily by the polyphenols and amides present in leaf extract, which in turn are oxidized
into a complex mixture of intermediates and byproducts [13]. The UV-vis spectra for AuNPs obtained with different gold (III)
concentrations are shown in Fig 1.

Fig 1. UV-vis spectra for gold nanoparticles for different Au(III) concentrations

No visible color change of the reaction medium or SPR peak was observed in 530 nm to 560 nm range when 0.51 mM- 1.27
mM of Au (III) concentrations were used for synthesis of AuNPs, possibly due to an extremely low rate of reaction. The reaction
medium changed its color from light yellow to light red only when Au (III) concentrations equal to or higher than 1.53 mM were
used. Repeated experiments revealed that 1.53 mM was the least gold (III) concentration required to synthesize AuNPs by using
aqueous oil palm leaf extract.
A broad SPR peak at 538 nm was observed with 1.53 mM gold concentration (Fig 2). Intensity of SPR peak increased with an
increase in gold precursor concentration. Increase in SPR peak intensity at higher precursor concentrationsis attributed to an
increase in formation of more gold nanoparticles [14]. Sharpness of SPR peak was also found to increase with an increase in Au(III)
concentration. Minor blue shift in SPR wavelength, from 538 nm to 536 nm was observed when precursor concentration was
increased from 1.53 mM to 4.055 mM indicating a reduction of mean particle diameter of the synthesized AuNPs [15].Size
reduction of AuNPs at higher precursor concentrations was confirmed with TEM image analysis as shown in Fig 5.

Fig 2. SPR spectra with different volume of Au(III) solution (1.53 mM)

Effect of volume of precursor (1.53 mM) added to the reaction medium containing a fixed volume of leaf extract was
investigated. SPR peak intensity increased when volume of precursor added was increased from 1ml to 3 ml. However, at precursor
volume higher than 3 ml, the SPR intensity decreased (Fig 3) possibly due to unavailability of sufficient amount of reducing
biomolecules in the leaf extract.
 Tausif Ahmad et al. / Procedia Engineering 148 (2016) 1396 – 1401 1399

Fig.3 Change in maximum absorbance with volume of gold solution

An increase in wavelength from 533 nm to 546 nm was observed when precursor volume was increased from 2 ml to 5 ml as
shown in Fig 4. The red shift was due to size enlargement with an increase in yield of gold nanoparticles [16].

Fig 4. Change in maximum wavelength with volume of gold solution

TEM images showed predominantly spherical and sparsely triangular shaped gold nanoparticle with average particles diameter
27.89±14.59 nm were formed with 1.53 mM gold solution as shown in Fig 5. Spherical, cylindrical, triangular, pentagonal and
hexagonal shaped gold nanoparticles were formed with average particle diameter 22.88±8.21 nm when 4.055 mM gold (III)
solution was used for synthesis as shown in Fig 5. The gold nanoparticles were well dispersed in the reaction medium without any
visible agglomeration. Our TEM results are in agreement with UV-vis SPR analysis. A minor blue shift observed in SPR (from
538 nm to 536 nm) was attributed to particle size reduction when higher precursor concentration (1.53 mM to 4.055 mM) was used
for AuNPs synthesis . TEM results also showed AuNPs size reduction from mean particle diameter 27.89 ±14.59 nm to 22.88
±8.21 nm when precursor concentration was increased from 1.53 mM to 4.055 mM, as shown below in Fig 5.

Fig 5. TEM images with (a) 1.53 mM (b) 4.055 mM Au (III) concentration
1400 Tausif Ahmad et al. / Procedia Engineering 148 (2016) 1396 – 1401

Dynamic light scattering (DLS) measurements indicated that the hydrodynamic diameter for AuNPs synthesized with 1.53 mM
gold solution was 55.22 ± 42.86 nm, as shown in Fig 6. The difference in particle diameter with TEM and DLS measurement
endorsed the fact that DLS measurements include thickness of biocompounds present on the surface of synthesized gold
nanoparticles.

Fig. 6 particles size distribution from DLS with 1.53 mM gold solution

FTIR analysis of the gold sol obtained after 60 min of reaction was performed to detect involvement of different functional
groups present in leaf extract. A broader peak observed at 3392 cm-1 is attributed the O-H bonds indicating presence of aromatic
alcoholic and phenolic compounds. Two more peaks were found at 1634 cm-1 and 1642 cm-1 corresponding to the presence of
amide groups. Smaller peaks observed at 1071 cm-1 ,1552 cm-1 and 1412 cm-1, 1370 cm-1, 1300 cm-1 confirmed the existence of
aromatic C-O bonds, N-H bonds and C-H stretching as shown in Fig 7 [17]. A major difference was witnessed for two peaks at
3392 cm-1 and 1634 cm-1 indicating contributory roles of O-H and C=O bonds in reduction of gold (III) ions to gold atoms. Hence,
phenolic, alcoholic and carboxylic compounds were considered to be accountable for reduction and stabilization of AuNPs [18].

Fig. 7 FTIR spectra for oil palm leaves extract and reaction solution

3. Conclusion

Gold nanoparticles were successfully synthesized by using aqueous oil palm leaves extract without addition of any reducing
and stabilizing agent. Effect of gold salt concentrations (0.51 mM – 4.055 mM) on size and morphology of gold nanoparticles was
investigated. A slight reduction in size of gold nanoparticles (27.89 ±14.59 nm to 22.88 ±8.21 nm) was observed with use of 1.53
mM and 4.055 mM gold concentrations respectively. Red shifting of SPR wavelength and AuNP size enlargement were detected
when larger volume of gold precursor solution was used for synthesis of gold nanoparticles. Phenolic, alcoholic and carboxylic
compounds present in leaf extract were responsible for reduction and stabilization of the synthesized gold nanoparticles.

Acknowledgements

This study was financially sponsored through FRGS (0153AB-I96) by Ministry of Higher Education Malaysia. The financial
support through STIRF (0153AA-C77) is also acknowledged. The Author Tausif Ahmad acknowledges the opportunity provided
by Universiti Teknologi PETRONAS Malaysia to pursue his PhD in Chemical Engineering.
 Tausif Ahmad et al. / Procedia Engineering 148 (2016) 1396 – 1401 1401

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