Materials Today: Proceedings xxx (xxxx) xxx

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Materials Today: Proceedings

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Preparation of amorphous oil palm frond ash (OPFA) via acid leaching
treatment as precursor for silica synthesis
Nor Surayah Osman, Norzahir Sapawe ⇑
Universiti Kuala Lumpur Branch Campus Malaysian Institute of Chemical and Bioengineering Technology (UniKL MICET), Lot 1988 Vendor City, Taboh Naning, 78000 Alor
Gajah, Melaka, Malaysia

a r t i c l e i n f o a b s t r a c t

Article history: Oil palm frond (OPF) was investigate in this study that aim to establish the potential of OPF as precursor
Received 14 February 2020 for silica synthesis. OPF is one of abundance biomass produce in oil palm plantation during pruning and
Received in revised form 7 May 2020 replanting phase that usually underutilized comparable to other oil palm-based waste. In this study, OPF
Accepted 9 May 2020
was first combusted at 600 ℃ to produce the oil palm frond ash (OPFA) that subsequently followed with
Available online xxxx
acid leaching treatment using 3% citric acid solution. The non-leached ash and leached ash was analysed
and characterized using Fourier Transform Infrared Spectroscopy (FTIR) and AAS Atomic Absorption
Keywords:
Spectroscopy (AAS). Combustion of OPF indicate that it produces approximately of 3.5% of ash out of total
Oil palm frond (OPF)
Acid leaching treatment
weight of OPF. The AAS analysis perform display a significant reduction of metal ions such as K+, Ca+ and
Silica Mg+ and total removal of iron from which proven the beneficial of acid leaching treatment in removing
Metal ions the undesired substance from OPFA. FTIR characterization display a significant different in spectra of
treated and non-treated ash and it also successfully illustrate that the OPFA produce contain the required
silica as well as the acid leached OPFA is in amorphous form due to the absence of band which indicating
the presence of tridymite (crystalline phase).
Ó 2020 Elsevier Ltd. All rights reserved.
Selection and Peer-review under responsibility of the scientific committee of the 4th International Con-
ference on Green Chemical Engineering and Technology: Materials Science.

1. Introduction
Elaies guineensis Jacq or commonly known as oil palm is the cur-
rent biggest plant-based oil producer in the world that reach one-
third or 31.3% from total global production according to Oil World
2018 report [1]. From this figure, Malaysia produce a total of 19.5
million tonnes which represent 27.7% of total palm oil world pro-
duction in 2018 [2]. This signify Malaysia position as the world sec-
ond largest palm oil producer in the world after Indonesia. From
MPOB statistic data, oil palm plantation in Malaysia has reached
5.85 million hectares in 2018 [2]. Vast production of palm oil in
Malaysia also lead to substantial figure of oil palm biomass (agri-
cultural waste) which is including oil palm frond (OPF) and oil
palm trunk (OPT) that generated during planting and pruning in
plantation site; empty fruit bunch (EFB), palm kernel shell (PKS),
mesocarp fiber (MF) and palm oil milling effluent (POME) produce
during palm oil extraction in the mill site [3,4].
⇑ Corresponding author.
E-mail address: norzahir@unikl.edu.my (N. Sapawe).
Oil palm frond or OPF is one of main oil palm biomass produce
in the plantation site that available throughout the year due to the
pruning and new planting activity. Loh (2016) tabulate based on
previous study data; approximately 10.40 tonnes (dry weight) of
OPF produced per hectare of plantation during pruning and
roughly 14.47 tonnes (dry weight) per hectare produced during
replanting [5]. According to Hamzah et al. (2019), about 51.19 mil-
lion tonnes of oil palm waste produced where 75% from this value
is represent by OPF and OPT [3]. Conventionally, OPF are decom-
posed for soil fertilization and erosion control aside shredded for
ruminant feed. Recent studies on OPF focus on its use as fuel/en-
ergy source (Hamzah et al., 2019; Loh, 2016) aside other prospects
including bio-gas, bio-char, bio-oil, bio-fertilizers, bio-composite
and briquettes [3–5]. Nonetheless, OPF full potential is still much
under-utilized where current trend of research heavily emphasis
on other oil palm biomass such as EFB, PKS and palm oil fuel ash
(POFA), that produces from boiler combustion in the mill plant.
Roslan et al. (2014), investigate properties of oil palm frond
properties suitability for utilization as biomaterials and biofuels
sources [6]. Yet, this study suggesting another interested finding

https://doi.org/10.1016/j.matpr.2020.05.333
2214-7853/Ó 2020 Elsevier Ltd. All rights reserved.
Selection and Peer-review under responsibility of the scientific committee of the 4th International Conference on Green Chemical Engineering and Technology: Materials
Science.

Please cite this article as: N. S. Osman and N. Sapawe, Preparation of amorphous oil palm frond ash (OPFA) via acid leaching treatment as precursor for
silica synthesis, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.333
2 N.S. Osman, N. Sapawe / Materials Today: Proceedings xxx (xxxx) xxx
which explain the present of silica in the OPF. This finding open an
avenue of research on the possible silica extraction from OPF. In
current setting, there is no study yet has been released on the
preparation of silica from OPF aside a few studies which utilized
oil palm ash (OPA) as silica sources [7,8]. Silica is well known as
one of valuable inorganic material that has variance usage and
application in scientific and another related field with projected
market of 8.8 billion USD by 2020 [9]. Nonetheless, current silica
sources come from conventional sources are expensive which open
avenue for possible economic silica precursor from waste material
such as agricultural waste [10,11]. This study aims to establish the
potential of OPF as one of agricultural waste that can be utilized as
silica sources.
Aside of that, this study also aims to prepared amorphous ash
that contain less impurities or the presence of other oxides that
usually associate with agricultural waste ash. For this purpose, acid
leaching treatment has been chosen as the method of ash treat-
ment. From their study, Faizul et al. (2013), display that oil palm
ash contain about 46% of silica that can be further purified up to
90% via acid leaching treatment [8]. Acid leaching treatment is
the most applied method in silica extraction which widely used
either in the standard silica extraction from the known source of
silica such as quartz and sand that has also extend to the extraction
of silica from agricultural waste ash such as rice husk, rice straw
and other. Strong acid such as HCl (hydrochloric acid), H2SO4 (sul-
phuric acid) and HNO3 (nitric acid) are usually used in acid leach-
ing. However, several studies have discovered that organic acid
such as citric acid can replace the invasive and harmful strong acid
in acid leaching treatment for silica preparation from agricultural
waste. Umeda and Kondoh study, successfully produce high purity
amorphous ash as silica precursor from rice husk ash via acid
leaching treatment using citric acid in 2008 and this study
repeated by Faizul et al. in 2013 that successfully produce amor-
phous ash from OPA [8,12]. The treated ash in Faizul et al. (2013)
study has the purity of 92% when prepared in optimum conditions
of temperature, reaction time and citric acid condition.
2. Methodology
2.1. Material
Oil palm frond (OPF) was collected from private palm oil plan-
tation at Alor Gajah, Melaka. The ash of OPF is treated using citric
acid (HmBG).
2.2. OPF preparation
The collected OPF is clean, sorted and cut to manageable size.
The OPF dried in the oven at 40 °C for 24 h.
2.3. OPF ash preparation
The OPF ash was prepared through combustion in electric muf-
fle furnace at 600 °C for 3 h. The weight before and after combus-
tion was properly measured.
2.4. Acid leaching treatment
OPF ash treated via acid leaching treatment modified from the
method describe in Faizul et al. (2013). OPF ash was weighed
approximately 20 gm on analytical balance and pour into 3% citric
acid inside a beaker. This mixture was placed on the hot place and
the temperature fix at 70 °C with 60 min reaction. The treated ash
was rinsed using distilled water at room temperature to remove
citric acid from the ash then followed with drying at 80 °C for
Please cite this article as: N. S. Osman and N. Sapawe, Preparation of amorphous oil palm frond ash (OPFA) via acid leaching treatment as precursor for
silica synthesis, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.333
8 h in the drying oven (model). Dried treated ash finally calcined
at 800 °C for 30 min in the electric muffle furnace.
2.5. Characterization study
OPF ash was characterized using Fourier Transform Infrared
Spectroscopy (Thermo Scientific Nicolet iS10) and AAS Atomic
Absorption Spectroscopy (Perkin Elmer AAnalyst 100).
3. Results and discussion
3.1. Preparation of oil palm frond ash (OPFA)
The main purpose of this study is to establish the potential of oil
palm plantation waste, oil palm frond (OPF) as silica sources which
later can be synthesized for further research and investigations.
Silica as one of highly stable inorganic material has wider applica-
tion in many scientific and related field which increased its current
demand. The current conventional process utilized high energy
consumption in producing silica which give impact to its price as
well as rising environmental problem. In tackling both issues, this
study utilized oil palm frond (OPF), the underutilized agricultural
waste from oil palm industries. OPF normally either discarded to
the landfill, burn or let rotten in the oil palm plantation which min-
imized its possible usage.
Thus, for this purpose, research design has been developed to
study this underutilized waste for its probable in silica extraction.
There are no data yet to be stablished and the undercurrent study
is developed by overlapping the current silica ash production
method from agricultural waste with certain modification to fit
the investigation purpose. The first step is obtaining the raw mate-
rial from the oil palm plantation and followed with cleaning and
drying process. The OPF was dried, cleansed and cut to manageable
size. The following process is 24 h drying in drying oven to remove
excess fluid. The final weight of the dried OPF taken prior combus-
tion at 600 ℃ for 3 h. This combustion rate is usually lower than
OPA (oil palm ash)/POFA (palm oil fuel ash) that produce from
combustion in the broiler in oil palm mill which usually between
temperature 900–1000 ℃ [13]. The difference in combustion
required can be explained based that OPA/POFA made up of
approximately 85% fiber and 15% other material that can be made
up from empty fruit bunch, palm kernel shell or other waste pro-
duce in oil palm milling process [12]. It is reported that material
with higher crystalline structure such as fiber will require more
energy to degrade as comparable to material with less of it [14].
A study made by Nordin et al. (2016) which characterize the com-
bustion rate of different part of oil palm fronds via thermo gravi-
metric analysis, used temperature between 50 and 800 ℃ under
nitrogen atmosphere which also lower than the temperature used
in broiler [15]. This study further proven, that dried OPF combus-
tion at 600 ℃ with duration of 3 h is adequate to produce the
required ash.
Subsequent processed followed with the combustion of OPF to
convert it into ash. Table 1 display the percentage of ash obtained
from OPF. From the sample prepared, 4000 gm of ash were com-
busted in laboratory electric muffle furnace. This combustion pro-
file shown that approximately 3.5% ash were collected from total
weight of dried OPF which indicate for every 100 gm of sample it
Table 1
Ash content from oil palm frond.
Oil palm frond (dry weight) Oil palm frond ash (OPFA) Ash content
(g) (g) (%)
4000 141 3.5
 N.S. Osman, N. Sapawe / Materials Today: Proceedings xxx (xxxx) xxx 3

in this leaching treatment is where the citric acid solution act as an

extraction media that will remove undesired substance from the
oil palm frond ash prior silica synthesis take place. From this pro-
cess, acid concentration has been chosen at 3% as it already dis-
plays the desire result in previous test perform accordingly and
the leaching process take place at 70℃ and for 6o minutes stirring
duration. For this treatment, atomic absorption spectroscopy (AAS)
analysis has been perform for the non-leached as and leached ash
to determine the removal of impurities from the oil palm frond
dash. As been state in other studies that utilized agricultural ash
waste, it is usually contain inorganic oxides such as magnesium
oxide, potassium oxide iron oxide and other. Table 2 shows the
chemical composition of selected AAS analysis before and after
Fig. 1. Ash obtained from oil palm frond. acid leached treatment.
From the tabulate results, it display how the present inorganic
oxide present before the leaching treatment is significantly reduce
Table 2 after the process, This proven how acid leaching is convenient as
AAS analysis result on leached and non-leached OPFA. pre-treatment prior to silica synthesis take place which beneficial
Non-leached OPFA (mg/L) Leached OPFA (mg/L) in removal of undesired substance in the ash. The utilisation of
organic acid such as citric acid as comparable to strong acid also
K 7.595 0.062
Mg 0.345 0.016 effective which provide an alternative in acid leaching treatment.
Ca 1.606 1.345 The removal of this inorganic oxide working based on the principal
Fe 0.002 – that the carboxyl groups of citric acid enabling the acid to acts as
the chelating agent where it can donate the protons (H+) that can
forming stable complexes with metal ions, consequently resulting
can produce 3.5 gm of ash. Based on study previously conduct by in their removal. From the table, the positively charged metal ions
Sapawe et al. (2018) the amount of ash produced by OPF is rela- such as potassium (K + ), calcium (Ca+) and magnesium (Mg+) is
tively higher than sugarcane bagasse (1.3%) and corncob (2.02%) reduced significantly after the acid leaching process, meanwhile
although it is lower than other agricultural waste tested, namely the iron content is totally removed.
bamboo culm (5%), banana leaf (13.38%) and bamboo leaf
(37.56%) [10,16]. Nonetheless, in this study sugarcane bagasse 3.3. FTIR characterization
ash contain the highest amount silica extracted (92.5%) which
indicate that amount of ash produced does not indicate the contain The oil palm frond ash also characterized using Fourier Trans-
of silica within the agricultural ash. Fig. 1 show the ash of oil palm form Infrared Spectroscopy (FTIR). Fig. 2 display the FTIR results
frond which is whitish gray in color and has light powdery texture of the treated ash, non-treated ash and the commercial SiO2 that
that associated with ash. recorded between wavenumber 4000–400 cm 1. From the FTIR
result, its exhibit significant difference in the spectra of treated
3.2. Acid leaching treatment of oil palm frond ash (OPFA) and non-treated ash which exhibit that FTIR spectra of acid leached
OPFA almost similar to the spectra of commercial silicon dioxide
OPFA obtained was treated by using acid leaching treatment (SiO2) The different in spectra of acid leached and non-acid leached
that modified from Faizul et al. (2013) study. The process involved prove the different of functional group present in both and Si ele-

Fig. 2. FTIR of non-treated ash, treated ash and commercial SiO2 (silicon dioxide).

Please cite this article as: N. S. Osman and N. Sapawe, Preparation of amorphous oil palm frond ash (OPFA) via acid leaching treatment as precursor for
silica synthesis, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.333
4 N.S. Osman, N. Sapawe / Materials Today: Proceedings xxx (xxxx) xxx
ment present is apparent in acid leached OPFA spectra as it bonds
with other ions.
The treated oil palm frond ash (red line) shown spectrum at
3420.94 cm 1 which could be ascribed as both Si-OH and OH-
vibrational bond in the structure. Similar broad peak also presents
in the non-treated ash and commercial silicon dioxide (SiO2). The
peaks at 1441.81 cm 1 representing the Si-OH stretching vibration
band meanwhile the peak at 1049.59 cm 1 bending vibration is
indicating of the Si-O-Si symmetric stretching and followed with
the peak 876.25 cm 1 which Si-O-Si asymmetric stretching vibra-
tions [15]. Peak observed at 466.26 cm 1 is for the bending vibra-
tions of Si-O-Si bond. This FTIR data also shows that the silica
phase of treated OPF ash is amorphous due to the absence of band
situated at 622 cm 1 which indicating to the presence of tridymite
(crystalline phase) that signify presence of cristobalite phase [17].
4. Conclusion
This study aims in investigate oil palm frond (OPF) as the pos-
sible source/precursor for silica synthesis with acid leaching treat-
ment utilized as a method of impurities removal that usually
present in agricultural ash waste. Initially this study, it shows that
OPF required a lower temperature as compare to the production of
OPA/POFA and for every 100 gm of OPF combust, it can produce
3.5 gm of oil palm frond ash (OPFA). The AAS analysis perform
display a significant reduction of metal ions such as K+, Ca+ and
Mg+ and total removal of iron from which proven the beneficial
of acid leaching treatment in removing the undesired substance
from OPFA. Meanwhile, FTIR characterization display a significant
different in spectra of treated and non-treated ash and it also suc-
cessfully illustrate that the OPFA produce contain the required sil-
ica as well as the acid leached OPFA is in amorphous form due to
the absence of band which indicating the presence of tridymite
(crystalline phase).
CRediT authorship contribution statement
Nor Surayah Osman: Formal analysis, Resources, Investigation,
Methodology, Writing – original draft. Norzahir Sapawe: Concep-
tualization, Data curation, Funding acquisition, Project administra-
Please cite this article as: N. S. Osman and N. Sapawe, Preparation of amorphous oil palm frond ash (OPFA) via acid leaching treatment as precursor for
silica synthesis, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.333
tion, Resources, Supervision, Validation, Visualization, Writing -
review & editing.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgements
The authors are grateful for the financial support by the Funda-
mental Research Grant Scheme (FRGS/1/2019/STG07/UNIKL/02/1)
from Ministry of Education Malaysia (MOE), the awards of Yayasan
Tengku Abdullah Scholarship (YTAS-Nor Surayah binti Osman),
and also the Universiti Kuala Lumpur Branch Campus Malaysian
Institute of Chemical and Bioengineering Technology (UniKL
MICET) for their support.
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