PRODUCTION AND CHARACTERIZATION OF FURANIC BIO-OIL FROM KAWAYAN

KILING (Bambusa vulgaris Schrad ex. Wendl) USING

MOLTEN CITRIC ACID IN AN OPEN SYSTEM

JOHN GODWIN A. MALLARI

(Project Leader)

RONNIEL D. MANALO
(Thesis Adviser)

DEPARTMENT OF FOREST PRODUCTS AND PAPER SCIENCE

(Implementing Agency)

DEPARTMENT OF SCIENCE AND TECHNOLOGY-

PHILIPPINE COUNCIL FOR INDUSTRY, ENERGY, AND EMERGING TECHNOLOGY
RESEARCH AND DEVELOPMENT (DOST-PCIEERD)
(Funding Agency)

01 MAY 2023 - 31 OCTOBER 2023

(6 months)
Summary Sheet

Project Title: Production and Characterization of Furanic Bio-oil from Kawaya

Kiling (Bambusa vulgaris Schrad ex. Wendl) using Molten Citric
Acid in an Open System

Project Leader: John Godwin A. Mallari

Implementing Agency: Department of Forest Products and Paper Science, College of

Forestry and Natural Resources, University of the Philippines
Los Baños

Project Source of Fund: PCIEERD-GIA

Total Budget: PhP 250,000.00

LIST OF TABLES
TABLE TITLE

2.0 The elemental and physical properties of bamboo species after

the pre-treatment

2.1 The ash content of P. amabilis and P. chino from age 1 to 3.

2.2 The chemical composition of bamboo fiber.

3.0 The Copper Strip Classification for Petroleum Products.

4.0 The Proximate Chemical Composition of Kawayan Kiling (B.

vulgaris).

4.1 The summary of the acquired yield of furanic bio-oil under three
(3) different time retention conditions

4.2 The summary of Physical Characterization of Furanic Bio-oil

under three (3) different time conditions.

4.3 The FTIR function groups found in the optimized furanic bio-oil.

4.4 The 10 chemical compounds with the highest amounts identified

in furanic bio-oil.

4.5 The proportions of individual-compound functional groups of

furanic bio-oil based on the identification from the GCMS
analysis.
 LIST OF FIGURES

FIGURE TITLE

2.0 The effect of MFA pretreatment on the product distribution of

microwave-assisted pyrolysis of raw and pretreated samples.

2.1 The product distribution (char, gas, bio-oil, and water-free bio-oil)
from (a) P. amabilis and (b) P. chino through pyrolysis at selected
maturation stages.

3.0 The weighted three (3) replicates of B. vulgaris flour for moisture
content determination.

3.1 The crucible with B. vulgaris flour placed in the furnace oven.

3.2 The set-up for extraction of organic solvents from B. vulgaris.

3.3 The set-up for the extraction of hot water extractives from B.
vulgaris.

3.4 The holocellulose preparation set-up.

3.5 The set-up for alpha-cellulose content determination.

3.6 The set-up for dewaxing the B. vulgaris meal flour.

3.7 The set-up for delignification of B. vulgaris meal flour.

3.8 The set-up for the alkaline treatment of B. vulgaris meal flour.

3.9 The experimental set-up for the production of furanic bio-oil: (a)
weighing of cellulose and citric acid; (b) cooking of the mixture;
(c) reduction of acetone through rotary evaporator; and (d)
extracted furanic bio-oil.

4.0 The B. vulgaris flour after subjecting to oven-drying for two (2)
days.

4.1 The obtained ash content from B. vulgaris after subjecting to

combustion for 30 minutes.

4.2 The Organic Extractives (Cyclohexane-Ethanol) of B. vulgaris

were obtained from Soxhlet Extraction. (a) Replicate; (b)
Replicate 2; (c) Replicate 3.
4.3 The oven-dried Organic Extractives of B. vulgaris: (a) Replicate
1; (b) Replicate 2; (c) Replicate 3.

4.4 The Hot Water Extractives of B. vulgaris after the Soxhlet

Extraction: (a) Replicate 1; (b) Replicate 2; and (c) Replicate 3.

4.5 The obtained Klason lignin from B. vulgaris: (a) Replicate 1; (b)
Replicate 2; and (c) Replicate 3.

4.6 The amount of holocellulose obtained from the

extractive-free meal flour of B. vulgaris.

4.7 The obtained alpha-cellulose from B. vulgaris: (a) Alkaline

Treatment of holocellulose of B. vulgaris; (b) the obtained
alpha-cellulose.

4.8 The trend in the yield of furanic bio-oil in relation to time

retention.

4.9 The interactions of citric acid in the cellulose: (a) in glycosidic

bonds; (b) in the oxygen of pyranose.

4.10 The hydrolysis of cellulose catalyzed by citric acid at 155 °C and

under open-system conditions leads to furanic bio-oil production

4.11 The FTIR Spectra of the three-hour produced furanic bio-oil.

4.12 The chromatogram of optimized furanic bio-oil at 300°C.

 1. INTRODUCTION

The continuous burning of fossil fuels imposes numerous threats to our environment
(Vasic et al., 2021). According to Cheng et al. (2015), its uncontrolled production utilizes
different global environmental and climatic constraints. Additionally, the carbon emissions
from fossil fuels in 2014 were considered the highest in history, amounting to 35.9 GtCO2
(Olson & Lenzmann, 2016). Consequently, these high concentrations of CO2 cause an influx
in our environment and atmosphere. Pollution (land, air, and water) has worsened in the past
decades. Such exorbitant air pollutants lead to the formation of acid rain, eutrophication, and
damage to crops and wildlife (Bertrand, 2021). Aside from these, land and water also suffer
from fossil fuel emissions (Khan et al., 2016). For instance, the extraction of fossil fuels
requires large land areas for infrastructure. The conversion of natural land destroys the
ecological balance, leading to wildlife fragmentation and biodiversity loss (Taylor & Tremblay,
2021). Besides environmental constraints, the socio-economic perspective is also affected
by excessive fossil fuel consumption. In Farrow et al. (2020) report, the over-usage of fossil
fuels accounts for 4.5 million deaths worldwide each year. Additionally, the estimated
economic loss worldwide is 2.9 trillion US dollars, or approximately 3.3% of the global GDP.

Further, several studies reported that the distribution of fossil fuels globally is uneven.
Based on the analysis of Martins et al. (2019), fossil fuels such as coal, natural gas, and oil
are considered to be nonrenewable sources of energy. Consequently, due to its limited
availability, the concern for energy security has become rampant in the past few years.
Likewise, the continuous depletion of fossil fuels should be eradicated and avoided as these
aid in the reduction of negative impacts on the environment, society, and economy (Martins
et al., 2019). Furthermore, the quest for renewable energy has been one of the significant
concerns in minimizing CO2 emissions and other harmful gases (Cheng et al., 2015;
Woyinbrakemi et al., 2021).

Meanwhile, the demand for alternative renewable energy has increased significantly
in the past years (Ma et al., 2016). For instance, biomass is the most abundant renewable
energy source (Kato et al., 2014). Aside from wind and solar power, the energy obtained
from biomass can be used in different forms, such as bioethanol, biodiesel, and bio-oil (Dai
et al., 2019; Cheng et al., 2015; Ma et al., 2016). More importantly, bio-oil production as an
alternative energy source is pivotal as this liquid synthetic fuel has numerous potential
sources of valuable chemicals (Cheng et al., 2015). Furthermore, to utilize and obtain bio-oil,
different technologies can be applied. For instance, thermochemical degradation can be
used, specifically in pyrolysis (Dai et al., 2019). Conversely, Romeo et al. (2020) reported
that the application of pyrolyses, such as the reactor systems and severe conditions,
restricts the scalability of the process together with factors such as the formation of
by-products. Specifically, the typical by-products of pyrolysis are biochar, gas, and tar.
Moreover, Park and Choi (2019) reiterated that using pyrolysis has remarkably higher energy
costs than using an open system.

In the study of Romeo et al. (2020), it was mentioned that the use of molten citric
acid is more efficient than pyrolysis. In fact, the application of this method does not utilize
potent inorganic compounds, harsh conditions, and enzymatic treatments. Additionally, the
employment of molten citric acid in bio-oil production does not produce by-products similar to
pyrolysis (Zhao et al., 2018). Correspondingly, bio-oil production in furanic-based has
become a point of interest in recent years (Gandini et al., 2016). According to Zhao et al.
(2018) and Romeo et al. (2020), furan is a member of bio-privileged molecules, which can
be transformed into other essential compounds with high added value. Likewise, furanic
compounds can be manipulated or directly used for crucial processes. For instance, the
dehydration of C6 carbohydrates can form 5-hydroxymethylfurfural (HMF) (Kohli et al.,
2019). Moreover, HMF is considered a vital biorefinery building block since this compound is
crucial for synthesizing several valuable chemical intermediates and liquid fuels (Zhao et al.,
2018 & Romeo et al., 2020).

However, previous studies focus only on converting cellulose to furanic bio-oil from
timber biomass, grass biomass, agricultural residues, and some algae (Bae et al., 2011, as
cited by Cheng et al., 2015). The production and characterization of furanic bio-oil from
bamboo have not been studied purely, and the application of furanic-based bio-oil from
bamboo is limited (Cheng et al., 2015). As a matter of fact, Bamboo, also known as poor
man’s timber, is considered one of the diverse non-timber species in the forest. In the study
by Yeasmin et al. (2014), 1 400 species of bamboo are distributed worldwide, and most of
them are fast-growing (Scurlock et al., 2000). Compared to hardwood species, bamboo has
a shorter felling period (between 3 to 5 years) (Li et al., 2007). Additionally, the natural
distribution of bamboo can mostly be found in the tropical, subtropical, and mild temperate
zones of the world (Mohanan & Liese, 1990). In the Philippines, there are between 60 to 62
species of bamboo can be found (Espiloy, 1996; Rao & Rao, 1998). Specifically, out of the
60 to 62 species, 21 are endemic or native in the Philippines. Furthermore, there are 13
species classified as climbers, while there are eight (8) species classified as erect (Rao &
Rao, 1998).

On the other hand, when it comes to chemical components, bamboo, and wood have
comparable amounts of chemical constituents (wood has 62-79% of holocellulose and
18-36% of lignin, while bamboo has 50-70% of holocellulose, 30% pentosans, and 20-25%
lignin) (Cheng et al., 2015). Therefore, these chemical components of bamboo indicate its
potential as a source of biomass for bio-oil production. Specifically, bio-oil production has
many applications, such as adsorbents, coatings, batteries, drug delivery, bio-pesticides,
polymers, corrosion inhibitors, and high-calorific biofuels.

Furthermore, with bio-oil applications, it is necessary to characterize its physical and

chemical properties. According to Zhang et al. (2013), the characterization of bio-oil is
important in order to identify the important organic chemicals, which is beneficial for biofuel
production. For instance, Zhao et al. (2018) reported that furanic bio-oils are crucial to the
synthesis of a series of valuable chemical intermediates and liquid fuels. Particularly, this
includes liquid fuel such as 2,5-furan dicarboxylic acid (FDCA), 2,5-dimethyl furan (DMF),
and levulinic acid (LA). Moreover, the organic compound 2,5-dimethyl furan or DMF can be a
useful additive in current petroleum. On the other hand, the hydrogenation of levulinic acid,
or LA can be upgraded to fuel additives and jet fuels (Zhao et al., 2018). Hence, with these
specified potential applications of bio-oil, it is of great importance in developing an efficient
and economical production system of bio-oil, specifically furan-based bio-oils (Zhang et al.,
2013; Zhao et al., 2018).

Nevertheless, the use of bio-oil in the industry can potentially reduce the emission of
greenhouse gases. In the study of Petterson et al. (2022), replacing fossil fuels with bio-oil
showed a decline in GHG emissions up to 0.24 MtCO2-ep/yr. Moreover, the production of 6.8
to 8.1 Mt of bio-oil could potentially reduce the carbon emissions of 8.6 to 10.3 MtCO2-eq/yr.
Overall, furan-based bio-oil is highly applicable to the sectors with higher demand for oil
quality, such as the transport sector and the petrochemical industry.

2. REVIEW OF LITERATURE

2.1. Consumption of Fossil Fuels

The consumption of fossil fuels is essential to the daily lives of humans. It is one of
the necessities needed to survive. According to Wang et al. (2022), many people would not
ignore the pivotal role of fossil fuels in this modern world since most economic activities
greatly depend on energy consumption. Furthermore, fossil fuel energy consumption is
considered the backbone and oxygen of economic development (Kalim et al., 2021).
Specifically, energy usage is an input that determines output production. Therefore, to fulfill
the demand, most countries globally, for instance, Brazil, Russia, India, China, and South
Africa, usually opt to use non-renewable energy sources rather than renewable sources of
energy (Wang et al., 2022). According to Ummalla and Goyari (2020), non-renewable energy
is the type of energy that produces harm to the environment. Likewise, most countries
generally choose to consume fossil fuels, increasing every year (Zahid et al., 2021).

Following the evolution of energy from wood to coal, gas, and petroleum, the energy
demand increased in the past years. In the study of Zou et al. (2016), the sustained increase
in economic and social needs will be inevitable in the succeeding years as industrialization
and development will be prominent. Correspondingly, in the last decades, the worldwide
consumption of energy has soared exponentially. For instance, in 1995, carbon dioxide
produced from fossil fuels was 8,588.9 million tonnes (Mtoe). Conversely, in 2015, the
amount of carbon dioxide emitted became 13,147.3 million tonnes (Mtoe) (Ahmad & Zhang,
2020). Moreover, petroleum is the most used fossil fuel, accounting for 40.8% of total energy
consumption. Petroleum is followed by natural gas, which accounts for 15.5% of the world's
energy consumption, and lastly is coal, accounting for 10.1% (Bimanataya & Widodo, 2017).

Additionally, countries such as Brazil, Russia, India, China, and South Africa have an
excessive proportion of coal, oil, and gas consumption due to the high public demand (Wang
et al., 2022). For instance, these countries' total produced GHGs and carbon dioxide were
5,217 metric tons in 2019, compared to 1,761 metric tons in 1990. Specifically, there is a
77.5% increase in oil consumption from these countries. Records found that China
consumed 1,138 metric tons of oil in 2019 compared to 641 metric tons in 1990 (Wang et al.,
2022). Following China is India, which utilized 224 metric tons of oil in 2019.

In terms of natural gas, Singh et al. (2022) reiterated that 910 billion cubic meters of
gas were used in 2019 compared to 506 billion cubic meters in 1990. As a matter of fact,
there has been a 79.84% increase in natural gas consumption over the past decades.
Specifically, Russia and China are the two countries that use the most natural gas globally.
For instance, the former consumes 501 billion cubic meters within a year, which is more than
half of the total gas consumption of the other countries. In contrast, the latter consumes 304
billion cubic meters of natural gas (Wang et al., 2022 & Singh et al., 2022).
 Aside from oil and natural gas, coal is also one of the most consumed natural gases.
Coal is a type of non-renewable energy since it takes millions of years to form. Likewise, it is
a combustible black or brownish-black sedimentary rock that contains a high amount of
carbon and hydrocarbons (US Energy Information Administration, 2021). In the study
conducted by Wang et al. (2022), it was found that China is the biggest coal consumer. The
country used up 3,826 metric tons of coal as of 2019. In comparison with South Africa,
Brazil, Russia, and India, the total coal consumption of these countries is 5,217 metric tons.
Therefore, the coal consumption in China is more than half of the total consumption of the
four countries. In addition, the share of China in the growing consumption of coal in the world
reached 56% in 2020 (International Energy Agency, 2021).

Furthermore, entering the 21st century, fossil fuel consumption will be dominant, and
it will remain until the year 2040 (Wang et al., 2022; Bimanatya & Widodo, 2017). According
to Ahmad and Zhang (2020), the global energy transformation will set forth to double speed
in demand for load across the globe. As a matter of fact, the world's total energy demand in
2018 was 14,020 million tonnes of oil equivalent. Based on the prediction and models, the
energy demand for 2040 would rise to 17,487 million tonnes of oil equivalent (Ahmad &
Zhang, 2020). Additionally, Africa would be on the top of the list, having a 2.7% increase in
energy demand. Following Africa, Asia is the second continent in terms of energy demand,
with a 1.9% increase. Moreover, most energy demand comes from Asia, Europe, and Africa
(Ahmad & Zhang, 2020; Wang et al., 2022).

However, the increasing demand for fossil fuels has its limitations. For instance, fossil
fuels are non-renewable energy sources, which means these resources are not permanent
(Singh et al., 2022). According to Kuo (2019), the world's energy consumption increased by
2.3% in 2018. Consequently, the continuous increase in energy consumption has rapidly
depleted most non-renewable energy resources (Kuo, 2019). In fact, since the 1970s, many
environmentalists have warned that the overexploitation of fossil fuels would lead to
depletion (Kirsch, 2020).

Furthermore, it was evident that oil reserves were diminishing. According to Hund et
al. (2020), oil production in Russia and Saudi Arabia was limited in 2020 due to the decline
of petroleum reserves. Hence, Saudi Arabia considered re-evaluating its long-term strategy
for producing petroleum for the succeeding years (Kirsch, 2020). Additionally, Kuo (2019)
presented that fossil fuel reserves are on the brink of depression. For instance, if developing
countries continue to perpetuate fossil fuels, most of which will dissipate in less than 100
years. Oil reserves will be depleted in 2052, while the globe will lose the resources for gas
and coal in 2060 and 2090, respectively (Kuo, 2019).

Moreover, these predictions are dangerous to the point every country should
consider. Since most developing countries are heavily dependent on fossil fuels for their
economic development (Wang et al., 2022; Singh et al., 2022; Kuo, 2019), nonetheless,
without the energy transition, the emissions of CO2 would grow up by two-thirds, or 60 billion
tonnes of CO2 per year (Energy Transition Commission, 2017). Alongside the emission of
CO2, the continuous depletion of our non-renewable resources would be prominent, affecting
many developing countries. Additionally, Zahid et al. (2021) pointed out that emitted gases
by burning fossil fuels have detrimental effects on our environment.
2.2 Effects of Fossil Fuels

Environmental Impacts of Fossil Fuels

The dependence of developing countries on fossil fuels has significant implications

for the environment. For instance, the carbon dioxide and other greenhouse gases emitted
by fossil fuels are the major contributors to global warming (Bimanatya & Widodo, 2017). In
addition, as stated in the study by Martins et al. (2019), the use of fossil fuels is the primary
contributor to environmental constraints, such as land, water, and air pollution. Moreover, the
three primary fossil fuels responsible for the degradation of the environment are coal, crude
oil, and natural gas (Hao et al., 2019). Correspondingly, the production and burning of these
fuels have far-reaching impacts on the environment. Such fossil fuels release methane,
mercury, sulfur dioxide, nitrogen oxides, and other toxic gases. Consequently, it will increase
the concentrations of toxic gases in the atmosphere (Hao et al., 2019 & Martins et al., 2019).

Furthermore, among the three fossil fuels mentioned above, coal has the most
destructive impact on environmental degradation since its extraction process damages
ecological stability and produces a metabolic rift (Hao et al., 2019). Metabolic rift pertains to
the differentiation between social metabolism and natural metabolic processes. Moreover,
human activities concerning economic growth have irreversible consequences on the
environment and damage the human-nature relationship (Austin & Clark, 2012).

Additionally, coal extraction destroys the habitat of many indigenous species and
natural stands, which causes environmental pressure. For example, the residues produced
in the extraction accumulate in the dams (Hao et al., 2019). Consequently, this scenario
enhances disasters, such as massive flooding and landslides. Moreover, coal production has
depleted most soil nutrients, damaged deep wells, degraded numerous landscapes, and
introduced toxic chemicals to rivers, affecting water quality (Hao et al., 2019 & Johnsson et
al., 2018).

In terms of crude oil production, it is inherently invasive to the world’s ecosystem.

Crude production involves exploration, drilling, and extraction and one of the significant
detrimental effects of these processes is deforestation (Hao et al., 2019). Aside from
deforestation, Hao et al. (2019) highlighted that crude production generates solid and liquid,
toxic chemicals that flow into different bodies of water, which contaminates the water quality.
Additionally, these poisonous chemicals accumulate in diverse landscapes, thus affecting the
microorganisms and other minerals in the soil. Furthermore, in the study of Johnston et al.
(2019), upstream crude oil extraction occurs near cities and urban areas.

Consequently, the operation of oil influences the nearby communities negatively. For
instance, oil extraction has adverse effects on soil, water, and air. In the case of air pollution,
the pollutants came from the hydrocarbons emitted from wells and pieces of machinery (Hao
et al., 2019). Besides the air pollution, reports found numerous oil spills that have deleterious
and long-term impacts on the ocean (Johnsson et al., 2018). Such oil spills have harmed
marine organisms, specifically planktonic organisms and other benthic organisms (Saadoun,
2015).

Additionally, coral reefs are also at risk of the effects of oil spills. According to
Perkol-Finkel and Benayahu (2007), coral reefs are essential nurseries for numerous fish
species and crustaceans. However, oil spills endanger marine animals due to exposure to
toxic substances and smothering. Furthermore, Saadoun (2015) found that dispersed oil is
harmful to soft and hard coral species during their early life stages. Therefore, oil spills
negatively influence the growth and development of coral reefs. Moreover, Shafir et al.
(2007) reiterated that since coral reefs are sensitive to oil spills, the assays indicated the
harmful effects not only to the coral itself and the neighboring organisms in the ocean.

Consequently, continuous industrialization in developing economies to suffice the

production of goods and satisfy the demands of the growing population is inevitable for such
progressive nations (Hanif, 2018). Correspondingly, the advancement of technologies and
other innovations resulted in new challenges, such as increasing demand for energy, loss of
natural resources, and carbon emissions (Azevedo et al., 2018). For instance, the waste
produced by East Asia and the Pacific was estimated to be 760,000 tons per day. Based on
the projection of Huaman and Jun (2014), the waste products in these regions would
intensify by up to 18 million tons per day in the year 2025. Consequently, this would also
surge the carbon emissions, causing different environmental catastrophes.

Moreover, global carbon dioxide production was reported to be 75% of the total
greenhouse gas emissions, and these gases do not dissipate quickly (Hanif, 2019).
Specifically, GHGs move from one zone to another; hence, pollutants have circulated in the
biosphere for thousands of years. As a result, the stored carbon in the atmosphere is
absorbed by seawater, converting it to carbonic acid. Furthermore, the sea waters become
acidic and damage the coral reefs and other marine animals (Azevedo et al., 2018; Huaman
& Jun, 2014). Nevertheless, fossil fuels do not cause pressure only on the environment. In
fact, fossil fuels also impose detrimental effects on socioeconomic aspects, such as acute
health problems and slow economic development (Hanif, 2018; Hao et al., 2019).

Socio-Economic Impacts of Fossil Fuels

Fuels are considered to be one of the necessities that are used to fill the needs of
society. During the latter part of the 20th century, the rapid development of fossil fuel
extraction frequently occurred near human settlements (Johnston et al., 2018). Furthermore,
there are around 70,000 oil fields across the world with approximately 1600 billion barrels of
known crude oil reservoirs (Johnson et al., 2018; Bentley, 2002). However, these oil fields
are concentrated near human populations and impose a significant impact on their health
and wellness. In fact, O’Callaghan-Gordo et al. (2016) reported that over 600 million people
worldwide are affected by fossil fuel production and extraction. Furthermore, the common
health diseases faced by humans due to the excessive burning of fossil fuels include
asthma, cancer, heart disease, lung diseases, and premature death (Bertrand, 2021).
Similarly, the combustion of a number of additives that can be found in fossil fuels, such as
benzene, toluene, ethylbenzene, and xylene, produces carcinogenic particles and aromatic
hydrocarbons that are harmful to the human body (Bertrand 2021; O'Callaghan et al., 2016).

Additionally, the study of Johnston et al. (2018) revealed that four (4) countries in
South America with at least 20 years of fossil fuel production portrayed an excessed risk of
cancer incidence. For instance, childhood cancer, such as hematopoietic cancer (blood stem
cell) was found to be increasing over the past years. Another leading cancer incidence was
found in children less than 14 years of age. Such a significant elevation of relative risk for
leukemia was observed among the children in Ecuador and most of them are living near
fossil fuel extraction sites (Johnston et al., 2018). Likewise, in the United States, specifically
in Colorado, it was reported that the occurrence of lymphocytic leukemia in children ages 5
to 24 was 4.3 times more likely to happen than in those who lived away from crude oil
refineries (McKenzie et al., 2017).

Overall, based on world statistics, the process of fossil fuel extraction and production
is the culprit for one in five deaths around the world (Bertrand, 2021). Moreover, the greatest
mortality impact of exorbitant fossil fuel production is estimated over the regions of Eastern
United States, Europe, China, India, and Southeast Asia (Schwartz et al., 2019).

In terms of the economic impacts, fossil fuels are considered to be the main
component of economic growth since most industries are run by fuels to function (Olson &
Lenzman, 2016). Hence, the intuition for the countries that are producing fuels would have
stable and improved economic development. However, the opposite occurs for those
countries specializing in fossil fuel extraction and production. Hao et al (2019) reported that
countries with heavy dependence on the extraction of fossil fuels may hinder economic
development, which can lead to reliance on unstable markets. For instance, Olson and
Lenzman (2016) reiterated that of the 34 countries that depend on their 5% of GDP from oil
production, only 9 are included in the most stable countries.

As a further matter, the economy of a country that is highly dependent on fossil fuel
exports has limited growth as compared to the countries that do not heavily rely on fossil fuel
production (Olson & Lenzman, 2016). Moreover, this phenomenon where countries are
overspecialized in one thing, such as fossil fuel extraction and production, is called resource
addiction (Hao et al., 2019). Consequently, the overspecialization of countries in one
resource has significant adverse effects on their economy. Instead of devoting to more
sustainable economic practices, heavy reliance on fossil fuels could potentially lead to rapid
economic loss (Olson & Lenzman, 2016; Hao et al., 2019). Furthermore, the reasons why
the economy of these countries fluctuated include the unpredictable global market, the loss
of competitiveness in some sectors, corruption, and failure to convert wealth into productive
assets (Hao et al., 2019).

In addition, the availability and distribution of fossil fuels around the world are at risk
of depletion. According to Bauer et al. (2016), it is anticipated that the world will run out of
fossil fuels in this century. For instance, the oil reserves will only last up to 50 years; natural
gas up to 53 years; and coal up to 114 years. Therefore, the limitation on fossil fuels
significantly increases their price on the world market.

In the study conducted by Shafiee and Topal (2008), the fluctuation of fossil fuel
availability will resonate with the fuel prices around the world. For instance, the continuous
decline of fossil fuel resources will raise the price of oil in the world market in the succeeding
years. Consequently, this phenomenon affects the international inflation rate, global GDP
growth, and other sectors heavily dependent on fuel consumption (Shafiee & Topal, 2008;
Hao et al., 2019; Olson & Lenzman, 2016). Hence, with the rampant increase of fossil fuel
prices, other commodities, such as food and other necessities will also increase. This
scenario will make the middle-class and lower-class societies have a hard time sufficing their
basic needs every day (Olson & Lenzman, 2016).
 Moreover, with the behavior of fossil fuels, the countries that are reliant on fossil fuels
will experience poverty and economic decline. For instance, Hao et al. (2019) reported that
continuous fossil fuel production contributes to a high level of environmental intensity,
causing environmental costs that harm people’s lives and their source of livelihood.
Nevertheless, the search for renewable and sustainable sources of energy is highly
suggested to lessen these adverse impacts on the environment, society, and economy.

2.3 Alternative Sources of Energy

During the 21st century, the demand for energy all around the world continues to
increase due to increasing population and industrialization. According to Owusu and
Asumadu-Sarkodie (2016), the world is becoming a global village as the requirement for
energy by all sectors across the nation increases. As a matter of fact, the demand for energy
by all sectors lies down to suffice the human social and economic needs, such as the
production of goods and services, food, and other necessities. Consequently, the security for
reserved energy in the future is one of the biggest challenges society faces. The continuous
depletion of fossil fuels has a significant impact on the availability of energy resources
around the world. Furthermore, Kaygusuz (2016) reiterated that 1.4 billion people around the
world lack access to electricity due to increasing prices and scarcity. Additionally, aside from
the energy scarcity and inflation rate, the continuous domination of fossil fuel-based energy
sources leads to the rapid growth of CO2 emissions (Kaygusuz, 2016; Owusu &
Asumadu-Sarkodie, 2016).

Correspondingly, to reduce the adverse effects of burning fossil fuels, the call for
alternative sources of energy to become rampant in today’s society. The consideration of
carbon dioxide as the major component of greenhouse gases (GHGs) is addressed to
reduce the emission from burning fossil fuels. In the study of Abolhosseine et al. (2014),
several policies and frameworks have been applied, such as the enhancement of renewable
energy employment. Likewise, renewable energy sources have the potential to displace the
harmful greenhouse gases from fossil fuel-based energy sources (Owusu &
Asumadu-Sarkodie, 2016).

Consequently, the different types of renewable energy sources include bioenergy,

hydropower, geothermal energy, solar energy, wind energy, and tide and wave energy
(Owusu & Asumadu-Sarkodie, 2016). Furthermore, these renewable energy sources are
labeled as clean and green energy sources due to their optimal use, reduction of waste, and
sustaining the environment based on the current economic and social needs (Edenhofer et
al., 2011).

As a further matter, the first type of renewable energy is hydropower. According to

Owusu & Asumadu-Sarkodie (2016), this type of energy is derived and harnessed from the
water moving from higher to lower elevations, with the aid of turbines to generate electricity.
On the other hand, direct solar energy refers to the renewable energy obtained from the
sun’s light. This type of energy uses photovoltaic and concentrating solar power to produce
electricity (Edenhofer et al., 2011). Another type of renewable energy would be geothermal
energy. This energy source is obtained from the earth’s interior as the heat energy source
(Owusu & Asumadu-Sarkodie, 2016). Moreover, other renewable energy sources, such as
wind energy and ocean energy; the former harnessed the kinetic energy from the wind
through the aid of windmills (Abolhosseine et al., 2014). On the other hand, the latter greatly
depends on the surface waves of the ocean when wind passes through the water. For
instance, the faster the wind, the stronger waves will be produced (Owusu &
Asumadu-Sarkodie, 2016).

Moreover, one of the important alternative sources of energy is biomass. According

to the Energy Information Administration (2022), biomass or bioenergy is a renewable
energy source derived from the organic matter of plants and animals. Similarly, biomass is
one of the pivotal alternative sources of energy since it can be used to produce biofuels (i.e.,
biodiesel, bio-oil, etc.) that can be substituted for fossil fuels (Owusu & Asumadu-Sarkodie,
2016). Aside from biofuels, biomass can be used for electricity generation, cooking, and
heating. Furthermore, the electricity generated from biomass has various sources, such as
forest by-products, agricultural residues, and animal husbandry residue (Abolhosseine et al.,
2014; Owusu & Asumadu-Sarkodie, 2016). Nevertheless, obtaining energy from biomass
has a significant effect on the reduction of waste products around the globe. For instance,
the materials needed to produce energy can either be a by-product, residues, or waste
products from the aforementioned sources (Owusu & Asumadu-Sarkodie, 2016). Hence, it is
a way to benefit society, such that it produces clean and sustainable energy and reduces the
production of waste.

2.4 Plant Materials as Source of Furanic Bio-oil

Parts of Plants that can be Source of Furanic Bio-oil

With the development of mitigation strategies for the impact of fossil fuels on the
environment and socio-economic development, the use of biofuels as a substitute for natural
gas, coal, and crude oil are being developed (Hood, 2016). Furthermore, biofuels obtained
from plants are considered the most abundant source of renewable energy since they
contain most of the essential chemical compounds needed to produce biofuels (Hood,
2016).

Correspondingly, the production of bio-oil has promising potential when it comes to

sustainable fuel production (Yu et al., 2011). However, to produce and utilize bio-oil, several
considerations should be made. For instance, the determination of plant parts from which
bio-oil can be obtained is necessary. Furthermore, the extraction of bio-oil can be obtained
from wood. In the study of Demirbas (2010), it was found that bio-oil can be produced from
wood. Based on the results of the study, the average liquid density of bio-oil was 1,195
kg/m3, as compared to the 750-990 kg/m3 for petroleum diesel fuels. Additionally, the yield of
bio-oil obtained from Picea orientalis ranges from 39.7% to 45.5%, depending on the
temperature applied. On the other hand, Chukwuneke et al. (2019) also conducted a study
on bio-oil production using the wood of Swietenia macrophylla (Mahogany). Based on the
results acquired, the bio-oil made from mahogany wood has a yield of 69.5% at a
temperature of 450℃.

Aside from the wood, other plant parts, such as the seeds can be a source of bio-oil.
Manimaran et al. (2020) reported that seeds of Trichosanthes cucumerina can be a good
source of bio-oil. In the study, the bio-oil was synthesized through the seed wastes of T.
cucumerina through solvent method extraction. Furthermore, the obtained bio-oil yield from
the seed wastes was found to be 28.40.4% under the temperature of 68℃. Moreover, the
study suggests that bio-oil obtained from the seeds of T. cucumerina manifests properties
similar to that of conventional fuel. Therefore, the accumulated bio-oil can be used as a
potential substitute for fossil fuels.

Apart from wood and seeds, leaves can also be a potential source of bio-oil. In the
study conducted by Thanigaivelan et al. (2021), the leaves of sugarcane were used to
extract essential bio-oils. Furthermore, the leaves were grounded until they became liquid in
form. Afterward, the liquid mixture was inoculated with Brewer’s yeast to extract the bio-oil
from the ground mixture. Moreover, the bio-oil yield from sugarcane leaves was found to
have a concentration of 1.59 at 72 hours of fermentation.

Moreover, most of the plant parts where bio-oil can be obtained are rich in
lignocellulosic materials, such as cellulose, hemicellulose, and lignin (Hood, 2016). These
lignocellulosic materials contained most of the stored energy obtained by the plants from the
sun. Therefore, the chemical components stored in these materials are produced generally
through the process of photosynthesis (Energy Information Administration, 2022; Owusu &
Asumadu-Sarkodie, 2016). Hence, the bio-oil can be obtained from these plant parts since
most of the chemical components found in this liquid energy can be obtained from wood,
leaves, and seeds (Demirbas, 2010; Manimaran et al., 2020; Thanigaivelan et al., 2021).

Lignocellulosic Materials

Lignocellulosic material is considered to be a natural resource that came from stems

or wood, leaves, and roots of trees consisting of brittle and fibrous tissues (Nakarmi et al.,
2022). Generally, these materials represent the dry part of the plant structures and
potentially can be utilized to produce renewable and sustainable energy (Romeo et al.,
2020). Furthermore, lignocellulosic materials are composed of cellulose, hemicellulose, and
lignin, which can be converted into fuels and other usable chemical compounds (Ragauskas
& Yoo, 2018).

Correspondingly, cellulose is a polysaccharide that is composed of a linear chain of

𝜷-1,4-glycosidic bonds and is considered to be the main component of lignocellulosic
materials (Romeo et al., 2020; Sun et al., 2016). Furthermore, cellulose is a stable
polysaccharide composed of 𝜷-D-glucopyranoses, which is approximately 5,000 to 10,000
units (Bellesia et al., 2010). Likewise, cellulose comprises amorphous and crystalline
portions, which are distributed randomly along the cellulose fibrils (Shi et al., 2012).
Additionally, the 𝜷-Glycosidic bond present in the cellulose allows the structure to form a
linear arrangement (Romeo et al., 2020; Bellesia et al., 2010).

On the other hand, hemicellulose greatly differs from cellulose since its structure is
characterized by short, branched chains of various sugars, such as glucose, mannose,
xylose, galactose, arabinose, 4-O-methyl glucuronic acid, and galacturonic acid units
(Romeo et al., 2020). Furthermore, hemicelluloses are also a significant component of the
plant cell wall (Gregory & Bolwell, 1999). Even though these components do not have
comparable commercial value, hemicelluloses play a significant role in the extraction of
cellulose (Bellesia et al., 2012; Gregory & Bolwell, 1999). In addition, hemicelluloses are
components that can be precipitated by ethanol following the extraction of the cell wall by a
diluted alkaline solution (Gregory & Bolwell, 1999).

Similarly, the third component of lignocellulosic materials is lignin. According to Deng

et al. (2016), lignin is the least abundant component of the lignocellulosic components,
having an average of 15% to 30% of the total mass. Furthermore, this polymer is composed
of phenylpropane units which are arranged in an amorphous, highly branched manner
(Romeo et al., 2020). Additionally, lignin is considered a complex hydrocarbon polymer,
consisting of aliphatic and aromatic constituents (Patel & Parsania, 2018). As a matter of
fact, lignin is a non-polar compound, which means it is insoluble to most solvents; hence, it
cannot be broken down into monomeric units (Deng et al., 2016; Zhao et al., 2018).
However, lignin can be removed from the lignocellulosic materials using different chemical
pretreatments. Consequently, this allows for milder and easier depolymerization of the
cellulosic materials in order to produce liquid fuels, such as bio-oils (Romeo et al., Dahunsi &
Enyinnaya, 2018). Moreover, lignin is soluble in hot alkali and can be oxidized easily. Also, it
is condensable with phenol but not hydrolyzable by acids (Patel & Parsania, 2018).

Cellulose as the Main Component of Furanic Bio-oil

Lignocellulosic materials are composed of cellulose, hemicellulose, and lignin

(Romeo et al., 2020). Among the three components, cellulose is the most abundant polymer
on earth, and the proper use and utilization of cellulose can contribute to the development of
sustainable and renewable energy, for instance, biofuels (Galiwango et al., 2019).
Furthermore, many studies have suggested the usage of bio-based renewable energy, such
as cellulose, can produce high-value chemicals, biofuel, polymer composites, and other
products similar to that of non-renewable energy resources (Kumar et al., 2017).
Additionally, Romeo et al. (2020) reinforced that cellulose-derived composites possess
high-value platform chemical compounds, which can be used for industrial applications and
refineries. As a matter of fact, one of the promising liquid fuels obtained from cellulose is a
mixture of compounds called bio-oil (Yin & Tan, 2012; Romeo et al., 2020).

Furthermore, Galiwango et al. (2019) reported that there has been a steady increase
in the utilization of cellulose due to its availability. As a further matter, cellulose has the
potential to be biodegradable, durable, non-toxic, and thermally and mechanically stable
(Prakash et al., 2018). Moreover, most of the chemical compounds found in bio-oil are
derived from cellulose (Yin & Tan, 2012). For instance, Galiwango et al. (2019) conducted a
study on the isolation of cellulose and 𝜶-cellulose from date palms, and based on the result,
it yielded about 74.70% to 78.63% of cellulose after the isolation process. Consequently, the
study suggested the isolation of cellulose from date palms has promising potential in the
production of bio-oil.

Additionally, Shi et al. (2016) also conducted a study on bio-oil production using
cellulose as the main component. Based on the acquired results, the reduction of crystallinity
and degree of polymerization of cellulose increases its surface, allowing the yield of
extracted bio-oil to increase. For instance, the maximum yield of bio-oil is 49.4% under five
minutes of time residence. Similarly, Romeo et al. (2020) also used cellulose-derived
materials to produce bio-oil. Consequently, the cellulose-derived materials yielded 60-80% of
bio-oil upon heating.

2.5 Production and Properties of Furanic Bio-oil

Different Production Processes of Furanic Bio-oil

In producing and extracting bio-oil from cellulose-derived materials, there are

numerous methods on how this liquid fuel can be obtained. Furthermore, the most common
process of bio-oil production is pyrolysis. According to Hu and Shi (2010), pyrolysis is a type
of thermochemical degradation where the biomass is decomposed into smaller molecules
through the application of thermal energy. Additionally, pyrolysis is considered to be a good
option to produce high-yielding liquid bio-oil (Cheng et al., 2015), which can be stored and
transported without compromising its quality. Moreover, pyrolysis is a thermochemical
process whereby the biomass is heated in the absence of oxygen (Inayat et al., 2022).

Furthermore, the use of pyrolysis can be categorized as slow, fast, and ultrafast. In
the case of bio-oil production, the commonly used pyrolysis is fast pyrolysis. In the study of
Inayat et al. (2022), fast pyrolysis usually occurs at a temperature of 450℃ to 700℃, with
heating rates of 1-200 ℃/s and a retention time of 20 seconds. Furthermore, the bio-oil
generated from fast pyrolysis is about 75% of the total products obtained from the process.
Moreover, Hai et al. (2020) investigated the potential of date palms in the production of
bio-oil. Consequently, the study revealed that the bio-oil obtained from the cellulosic
components of date palm yields a bio-oil that has a high viscosity and high heating value.
Nonetheless, it was suggested that the acquired bio-oil can be further refined and utilized in
biofuel applications (Hai et al., 2020; Bharath et al., 2020).

Aside from pyrolysis, bio-oil can also be obtained with the aid of acids. In the study of
Romeo et al. (2020), the produced bio-oil was obtained with the aid of molten citric acid in an
open system. Furthermore, the isolated cellulose was mixed with citric acid under the
specified temperature and retention time. The samples were heated based on the melting
point of citric acid. Afterward, the collected bio-oil was subjected to different test analyses,
such as FT-IR Analysis and Gas Chromatography-Mass Spectrometry (GC-MS) to
characterize its elemental, physical, and chemical properties.

As a further matter, the use of acid as an agent in producing bio-oil is more effective
than that of pyrolysis. In the study conducted by Isahak et al. (2012), the use of reactor
systems (closed systems) and severe conditions limit the functionality of the process of
producing bio-oil. For instance, the bio-oil produced from pyrolysis often has by-products,
such as biochar, humins, gas, and tar. Consequently, these side products sometimes
overpower the yield of bio-oil, leading to low-quality produced bio-oil (Isahak et al., 2012;
Guedes et al., 2018). Conversely, Romeo et al. (2020) reported the use of acid, such as
citric acid in bio-oil production would not result in the formation of by-products.

Additionally, apart from the pyrolysis and acid applications, bio-oil can also be utilized
through the use of hydrothermal liquefaction. According to Yin and Tan (2012),
high-temperature hydrothermal liquefaction (HTL) is regarded as one of the most promising
technologies for the production of biofuels because it can transform cellulosic biomass into
bio-oil. In this method, it uses hot-compressed water as the reaction medium, whereas the
wet biomass can be converted directly without prior pre-treatment (Demirbas, 2009).
Furthermore, the typical HTL process started with liquified biomass in order to produce liquid
products (Yin & Tan, 2012). Consequently, the bio-oil is extracted from the liquid products
through the use of organic solvents. However, the extraction step does not involve chemical
reactions; therefore, the bio-oil yield would be determined by the HTL reaction step (Xiu et
al., 2010).

Moreover, there are numerous methods and technologies on how bio-oils can be
utilized and produced. For instance, Romeo et al. (2020) reiterated that advancements in
bio-oil production can be attributed to these technologies, such as microwave irradiation, the
application of Lewis or Bronsted acids at high pressure and high temperature, and the
employment of concentrated marine seawater. In the case of microwave irradiation, Dai et al.
(2020) reported that a pre-treatment procedure, such as the use of formic acid, is utilized to
significantly decompose the biomass structure more quickly than conventional heating. On
the other hand, Zhao et al. (2018) mentioned that the application of Lewis acid and Bronsted
acid in bio-oil production can be undertaken in a low-boiling single-phase reaction system,
consisting of water and 1,2-dimethoxyethane. Furthermore, the applied Lewis and Bronsted
catalytic acids in the experiment were aluminum chloride (AlCl3) and phosphoric acid
(H3PO4).

Properties of Cellulosic Bio-oil

Depending on the methods applied, the properties of cellulosic bio-oil may vary. For
instance, in the study conducted by Dai et al. (2019), the microwave-assisted pyrolysis of
formic acid was used to produce and characterized the bio-oil from bamboo species. The
bamboo species were subjected to pretreatments under different temperatures. After this,
the effects on physical and chemical properties were determined (see Table 2.0).

Table 2.0 The elemental and physical properties of bamboo species after the pre-treatment.

Parameter MFA-130°C MFA-150°C MFA-170°C

Proximate Analysis (wt. %,db)

Ash Content 0.31 0.23 0.21

Volatile Content 92.16 91.07 88.23

Fixed Carbon Content 7.53 8.70 11.56

Ultimate Analysis

C 47.57 48.21 49.07

H 4.90 4.92 4.88

O 47.22 46.64 45.84

N ND ND ND
 Energy density 1.13 1.11 1.12

CrI (%) 52.19 58.83 63.81

Source: Dai et al. (2019)

Dai et al. (2019) obtained the following physical and elemental properties of
pre-treated samples of bamboo species. Based on the acquired results, the pre-treatment
procedure significantly decreases the ash content of the sample as well as the volatility.
Furthermore, the decrease in volatility can be attributed to the degradation of hemicellulose,
whereas the cellulose and lignin were slightly decomposed in the MFA pre-treatment (Zheng
et al., 2015). Additionally, the properties of bio-oil under pretreatment microwave irradiation
reduce its mass and energy yield (Dai et al., 2015). According to Huang et al. (2012), the
reduction of mass and energy yield by the samples is due to the decomposition of the
lignocellulosic materials vita dehydration and devolatilization at extreme temperatures.

Furthermore, Dai et al. (2019) also presented that conducting pretreatment

procedures on bamboo samples significantly reduces the yield of bio-oil (see Figure 2.0).

Figure 2.0 The effect of MFA pretreatment on the product distribution of microwave-assisted
pyrolysis of raw and pretreated samples.
Source: Dai et al. (2019)

The graph shows the yield of bio-oil under microwave irradiation together with the
byproducts. According to Dai et al. (2019), the bio-oil, gas, and char yields ranged from
26.45% to 32.14%, 44.63% to 56.89%, and 16.66% to 23.23%, respectively. Consequently,
based on the graph, it can be noticed that the yield of bio-oil and bio-char decreases as the
temperature of pretreated samples increases. According to Wang et al. (2014), the process
of MFA pretreatment resulted in the destruction of certain light components of the biomass,
which led to a reduction in the amount of bio-oil that could be extracted through continuous
pyrolysis. Moreover, Dai et al. (2019) reported that a subsequent increase in temperature
during the pretreatment process typically reduces the yield of bio-oil because high
temperatures increase the likelihood of excessive decomposition of biomass components.

Apparently, in the study of Cheng et al. (2015), the production of bio-oil was utilized
through fast pyrolysis. For instance, there were two (2) different bamboo species subjected
to bio-oil production, such as Pseudosasa amabilis and Pleioblastus chino. Additionally,
there were no pretreatments involved in the experiment. Furthermore, Cheng et al. (2015)
assess the effect of different ages of bamboo in the production of bio-oil. Consequently, as
the age of bamboo increases, the yield of bio-oil somewhat increases (see Figure 2.1).

Figure 2.1 The product distribution (char, gas, bio-oil, and water-free bio-oil) from (a) P.
amabilis and (b) P. chino through pyrolysis at selected maturation stages.
Source: Cheng et al. (2015)

Cheng et al. (2015) noted that bio-oil yield slightly increased in the case of P.
amabilis. For instance, the yield percentage ranges from 30% to 40%. On the other hand,
the yield of bio-oil for P. chino did not change significantly as compared to the first one.
Furthermore, the yield of water-free bio-oil somewhat increased as the bamboo aged.
According to Mourant et al. (2011), alkali and alkaline earth metals can reduce the organic
phase of bio-oil. Consequently, this leads to the increase of water in bio-oil. As a further
matter, in comparison to the findings of Dai et al. (2019), the yield in bio-oil was significantly
higher than those samples undergoing pretreatment. Contrarily, the ash content of the
samples that do not undergo pretreatment increases with age. Dai et al. (2019) reported that
the ash content of the samples declined with increasing temperature during the pretreatment
(see Table 1.0). However, Cheng et al. (2015) noted that the ash content of the bamboo
species escalated (see Table 2.1).

Table 2.1 The ash content of P. amabilis and P. chino from age 1 to 3.

Pseudosasa amabilis Pleioblastus chino

Parameter
1 year 2 year 3 year 1 year 2 year 3 year

Ash Content 1.03 1.17 1.38 1.06 1.46 1.79

Source: Cheng et al. (2015)

In the case of Romeo et al. (2020), the bio-oil was produced through the aid of
molten citric acid in an open system and the yield was about 60% to 80% of the total isolated
cellulose. Correspondingly, the maximum yield of bio-oil occurs at the melting point of citric
acid, which is 152℃ to 155℃. Additionally, there were no byproducts produced during the
extraction and process. Furthermore, Romeo et al. (2020) also presented the chemical
composition of bio-oil under different reaction times. For instance, some of the chemical
compositions present are 5-methyl furan, 2,5-bis (hydroxymethyl) furan, 2,5-furan
dicarboxylic anhydride, 5-formyl-2-furancarboxylic acid, 5-hydroxymethyl-2-furan carboxylic
acid, 5-hydroxymethylfurfural, glucose, and citric acid. Moreover, these chemical compounds
were produced during the time retention of 30 minutes, 1 hour, 2 hours, 3 hours, and 5 hours
(Romeo et al., 2020).

2.6 Bamboo as Source of Furanic Bio-oil

Species Distribution of Bamboo in the World

Bamboo, known as the poor man’s timber, is the general name for more than 1250 to
1662 species distributed worldwide (Cheng et al., 2015; Yeasmin et al., 2014; Canavan et
al., 2017). Furthermore, bamboo belongs to the family of Poaceae and the subfamily of
Bambusoideae (Nfornkah et al., 2020). According to Canavan et al. (2017), there are 121
genera of bamboo species across the globe and they have a wide variety of forms. For
instance, there are dwarf herbaceous species, which are commonly found in temperate
regions, while those tall, thick, and woody-like bamboo species that can grow up to 20
meters can be found in tropical countries, such as Southeast Asia (Bystriakova et al., 2004).

Furthermore, Yeasmin et al. (2014) reported that about 14 million hectares of the
earth's surface area are covered by bamboo, of which 80% of it belongs to Asia. As a matter
of fact, Brystraikova et al. (2003) reiterated that the major species richness of bamboo can
mostly be found in the Asia-Pacific region, followed by South America. However, the least
concentration of bamboo distribution can be found in the African region, while in Europe,
there have been no reported native bamboo species found. Additionally, the herbaceous
bamboo species constitute about 110 species around the world. Specifically, Yaesmin et al.
(2014) indicated that herbaceous bamboo can be found in the neotropics of Brazil,
Paraguay, Mexico, and the West Indies. On the other hand, the paleotropical woody bamboo
species are distributed in the tropical and subtropical regions of Africa, Madagascar, Sri
Lanka, Southern Japan, Southern China, and Oceania (Yeasmin et al., 2014).

Correspondingly, most bamboo species can adapt to a wide array of ecosystems and
climatic conditions (Canavan et al., 2017). For instance, bamboo species can be found in
diverse environments, such as moist deciduous forests, semi-evergreen forests, tropical and
subtropical forests, and temperate areas (Li & He, 2019). Furthermore, 80% or 900 bamboo
species under 65 genera are concentrated in Asia, specifically in China, Japan, and India (Li
& He, 2019; Yeasmin et al., 2014; Canavan et al., 2017). In addition, unlike hardwoods,
bamboo can regrow immediately after its harvesting, which means it can be harvested every
year (Li & He, 2019; Yeasmin et al., 2014). Consequently, bamboo is considered to be the
most important non-wood forest resource. Similarly, Li and He (2019) indicated that bamboo
represents the ideal wood substitute, and could effectively minimize the pressure on the
demand for timber and forest wood production.

Moreover, over the past few years, bamboo has gained popularity due to its
versatility (Canavan et al., 2017). For instance, bamboo is believed to be especially
important in meeting the current economic, environmental, and social needs (Hoogendoorn
& Benton, 2014; Liese & Kohl, 2015). Correspondingly, Song et al. (2011) reported that
commercially grown bamboos are more sustainable and renewable than the current crops
found in agricultural lands in terms of products and energy production. With this, the
potential for bamboo to be utilized in renewable energy production becomes interesting.
However, Cheng et al. (2015) reiterated that compared to the other types of biomass (i.e.,
agricultural residues, wood and wood wastes, algae, and animal husbandry), the utilization
of bamboo for biofuel production has not caught the attention. Therefore, Chaowana (2013)
suggested that sufficient studies regarding bamboo’s potential for renewable energy
production should be conducted.

Chemical Composition of Bamboo

Similar to hardwood species, bamboo is considered to be an essential and

renewable lignocellulosic resource for biofuel production (Chang et al., 2015). Therefore, the
utilization of bamboo for green energy production has increased significantly. Similar to
hardwood species, bamboo is also made up of lignocellulosic materials, such as cellulose,
hemicellulose, and lignin (Cheng et al., 2015). As a matter of fact, these three components
contribute to 90% of the total bamboo mass (Azeez & Orege, 2016). Furthermore, Li et al.
(2010) reported that the chemical composition of bamboo usually varies depending on the
species and their age. However, the general percentage of chemical composition in bamboo
is presented in Table 2.2.

Table 2.2 The chemical composition of bamboo fiber.

Chemical Constituents Percentage (%)

Cellulose 73.83

Hemicellulose 12.49
 Lignin 10.15

Aqueous Extract 3.16

Pectin 0.37

Source: Azeez & Orege (2016).

Correspondingly, the cellulose content of bamboo species decreases with the

increase in the age of bamboo (Azeez & Orege, 2016). Conversely, different studies show
the variation in the chemical composition of bamboo species. For instance, Sathisuksanoh et
al. (2010) reported that bamboo species located in Japan are mostly made up of 47%
cellulose, 23% hemicellulose, and 27% lignin. On the other hand, Kuttiraja et al. (2013)
found that Dendrocalamus sp is made of up 47% cellulose, 16% hemicellulose, and 18%
lignin.

In the case of Giant bamboo (Dendrocalamus asper), Leenakul et al. (2010) reported
that this species is made up of 41% cellulose, 27% hemicellulose, and 27% lignin.
Furthermore, Chang et al. (2015) reiterated that giant bamboo is the tallest among all the
bamboo species, and it is often used for food, construction, furniture, decorations, and other
purposes, such as biofuel production (Bonilla et al., 2010). Additionally, Chang et al. (2015)
revealed that the culm of giant bamboo is composed of saturated and unsaturated
hydrocarbons, including alkanes, alcohol, ketones, aldehydes, fatty acids, and minor
aromatic compounds.

Moreover, the chemical contents of bamboo were comparable to the hardwood

species. For instance, Cheng et al. (2015) described that hardwood species are mostly
composed of 62-79% of holocellulose and 18-36% lignin, while most bamboo species have
50-70% holocellulose, 30% pentosans, and 20-25% lignin. Therefore, bamboo has great
potential to be a source of biofuel production, specifically bio-oil (Li et al., 2007).

3. METHODOLOGY

3.1 Sample Preparation of B. vulgaris

Healthy mature poles of B. vulgaris were collected from the Bambusetum located at
the Los Baños Experimental Station in the Mt. Makiling Forest Reserve. The Bambusetum is
under the supervision of the Ecosystem Research and Development Bureau of the
Department of Environment and Natural Resources (ERDB-DENR), Los Baños, Laguna.
The samples of B. vulgaris were transported to the Department of Forest Products and
Paper Science, College of Forestry and Natural Resources. Furthermore, the delivered B.
vulgaris was already cut into matchsticks and stored in a transparent plastic bag.

Moreover, to conduct the proximate chemical analysis and the production of bio-oil,
the bamboo samples were ground using a Wiley mill to pass a 40-mesh screen.
Furthermore, the total weight of the produced bamboo flour was 357.0 g and kept in air-tight
plastic bags. Specifically, the bamboo flour was stored in three (3) air-tight containers with
the following weights 105 g, 132 g, and 120 g, respectively. Nevertheless, each plastic bag
was labeled as sample 1, sample 2, and sample 3.
3.2 Proximate Chemical Analysis of B. vulgaris

Moisture Content Determination. To determine the moisture content of the

samples, three (3) two (2) grams of bamboo flour were oven-dried in a tare petri dish and
labeled as K1, K2, and K3. Consequently, the initial weights of the three (3) bamboo
samples were determined and noted. Afterward, the samples were dried for 24 hours in an
oven at 103±2℃, then cooled in a desiccator for 15 minutes, and weighed on an analytical
balance. Furthermore, the samples were returned to the oven for another 24 hours, cooled,
and reweighed. Subsequently, repeated weighing was executed until constant weights were
reached. Moreover, the moisture content (%MC) was calculated based on the oven dry
weight.

Figure 3.0 The weighted three (3) replicates of B. vulgaris flour for moisture content
determination.

Ash Content Determination. To execute the ash content determination, clean, three
(3) empty crucibles were ignited in a muffle furnace at 600℃ for 30 minutes. Following the
ignition, the crucibles were slightly cooled and placed in the desiccator for about 15 minutes
and then weighed on the analytical balance. Furthermore, approximately two (2) grams of
bamboo flour were placed in every tarred crucible and labeled as K1, K2, and K3.
 Figure 3.1 The crucible with B. vulgaris flour placed in the furnace oven.

Afterward, the three (3) samples were ignited in a furnace at room temperature until
they reached 600°C. Correspondingly, the samples were allowed to remain at 600°C for 30
minutes and then allowed to cool in air. Thereupon, the cooled samples were placed inside
the desiccator for 15 minutes and then weighed. Moreover, the percent ash content was
calculated based on the oven-dry weight basis of the sample.

Cyclohexane-Ethanol Extraction. For the cyclohexane-ethanol extraction, two (2)

grams of oven-dried bamboo flour were weighed in Petri dishes and labeled S1, S2, and S3.
Furthermore, the Petri dishes with bamboo flour were transferred onto filter paper, wrapped,
and then tied neatly. Afterward, the samples were placed in the Soxhlet apparatus. The
extraction flasks were filled with 200 mL of cyclohexane-ethanol at a 2:1 volume-to-volume
ratio. The temperature of the hot plate was adjusted to provide a boiling rate that cycles the
solvent at least three (3) times per hour. Furthermore, the extraction was done over a 6-hour
period and then allowed to dry under the hood at least overnight.
 Figure 3.2 The set-up for extraction of organic solvents from B. vulgaris.

The extractive content was determined by removing the solvent in a vacuum using
the rotary evaporator. In fact, the round-bottom flask containing the solution was subjected to
rotary evaporation for at least 10 minutes. Furthermore, the samples were oven-dried until
the constant weight of the round bottom flask and extractives were attained. The percent
extractive content of cyclohexane-ethanol was acquired as a percentage of the oven-dried
weight of the bamboo flour.

Hot Water Extraction. In the case of hot water extraction, the filter paper containing
the extracted bamboo flour from cyclohexane-ethanol was then air-dried for two (2) to three
(3) days. Following the air-drying process, the three (3) samples were then placed in the
soxhlet extractor and about 200 mL of distilled water was added to the tared-weight
round-bottom flask. Afterward, the round-bottom flask was then placed on the hot plate.
Furthermore, the temperature of the hot plate was adjusted based on the boiling rate of
water, which cycled the solvent at least three (3) times per hour.
 Figure 3.3 The set-up for extraction of water extractives from B. vulgaris

Similar to the cyclohexane-ethanol extraction, the extraction for hot water also lasted
for six (6) hours. As a further matter, the three (3) filter papers containing the bamboo flour
sample were allowed to dry under the hood for at least 24 hours. Meanwhile, the three (3)
round-bottom flasks were removed from the soxhlet extractor, and the water in the flasks
was drawn out using the rotary evaporator. Nonetheless, the percent extractives for hot
water was calculated based on the oven-dry weight of the extracted bamboo flour.

Lignin Content Determination. Weigh about 1.0 g of the extractive-free B. vulgaris

flour and place it in a 50-mL beaker. Afterward, 10 mL of 72% sulfuric acid was gradually
added with the aid of a pipette. The addition of sulfuric acid is made in small increments
while stirring and macerating the material with a glass rod. Furthermore, the soaked,
extractive-free bamboo sample was left at room temperature for two (2) hours with
occasional stirring, for instance, stirring the sample every 15 minutes.

The mixture will be quantitatively transferred to a 1.0 L Erlenmeyer flask. Additionally,

distilled water from the wash bottle was used to rinse the beaker to remove any remaining
bamboo flour. The water acquired from washings was transferred to the 1.0 L Erlenmeyer
flask. In addition, distilled water was added to the mixture in order to dilute it until the desired
final volume of 300 mL was reached. The Erlenmeyer flask was placed on a hot plate set to
300 °C and covered with an inverted 50 mL Erlenmeyer flask. In order to maintain a constant
mixture volume, distilled water was added to the flask every 30 minutes while the flask was
heated for approximately 180 minutes.
 The insoluble lignin was extracted using vacuum filtration and pre-weighed fritted
glass crucibles. Additionally, the lignin was washed free of acid with 150 mL of hot, distilled
water (at 100 °C). After the vacuum filtration, the fritted crucibles containing the lignin were
dried in an oven for at least one (1) hour, then transferred to a desiccator for cooling.
Furthermore, the oven-dried samples were measured, and the percent lignin content was
calculated as the percentage of the oven-dry weight of the bamboo flour.

Holocellulose Content Determination. Prior to the actual experiment, the following

solutions were prepared, such as 250 mL stock solution A; which consists of 60 mL acetic
acid and 1.3 g NaOH per liter of distilled water), three (3) 100 mL of 20% sodium chlorite
solutions, 1% acetic acid solution. Moreover, prepare 1.0 L of distilled water and place it in
the freezer. Furthermore, weigh accurately three (3) 5.0 g of extractive-free B. vulgaris and
transfer each weighed bamboo flour onto a 100 mL Erlenmeyer flask. Afterward, add 30 mL
of stock solution A to each flask and place the flask in a constant temperature hot water bath
heated to 75 °C. Additionally, 3.0 mL of a 20% sodium chlorite solution was added to each
flask. Next, an inverted 25 mL Erlenmeyer flask was placed over each flask. Subsequently,
the same amount of sodium chlorite was added to each flask after 30 minutes, 60 minutes,
105 minutes, and 150 minutes. Moreover, the digestion of the extractive-free bamboo flour
continued for 195 minutes.

Figure 3.4 The holocellulose preparation set-up.

The flasks were removed from the hot water bath and the contents were transferred
to crucibles; whereas, the excess solution was removed by suction with the use of a
vacuum. Furthermore, each flask was rinsed with 60 mL of distilled iced water. Meanwhile,
the samples were washed with four (4) 75 mL quantities of 1% acetic acid solution and two
(2) 30 mL quantities of acetone or methanol, respectively. Afterward, the samples were
transferred to a Petri dish and allowed to air dry for at least 36 hours to reach equilibrium
moisture content, then obtain the final weight. Moreover, the percent holocellulose content
calculation was determined from the oven-dry weight of the extractive-free bamboo flour.

Alpha-Cellulose Content Determination. To accomplish the alpha-cellulose content

determination, weigh approximately three (3) replicates of 1.0 g of holocellulose obtained
from the holocellulose content determination, and place it in a 250 mL beaker. Add 20 mL of
a 15.6% sodium hydroxide solution that is free of carbonates (17.5 g of NaOH in 100 mL of
distilled water). Afterward, through the use of a glass rod, macerate the holocellulose of B.
vulgaris flour until it is thoroughly disintegrated and penetrated by the alkali solution. After
the disintegration, place a watch glass over the beaker and continue the reaction for 30
minutes at room temperature.

Figure 3.5 The set-up for alpha-cellulose content determination.

An additional 20 mL of distilled water was added to the mixture and transferred the
contents of each flask were to a fritted glass bottom crucible of about 30-35 mL capacity, and
with coarse porosity. Correspondingly, remove the excess solution by suction through a
vacuum and wash the sample with 250 mL of distilled water (20 °C). Following the washing
of the samples, disconnect the suction tube, add 20 mL of 10% acetic acid, and soak the
samples for five (5) minutes. Moreover, reconnect the suction tube and continue the suction
by washing the samples with 250 mL of distilled water (20 °C) until all excess acid is
removed. Furthermore, place the fritted glass into an oven with a maintained temperature of
105 °C for at least 24 hours. Consequently, the calculation of the percent alpha-cellulose
was based on the oven-dry weight of the samples.
3.3 Production and Isolation of Cellulose from B. vulgaris

Dewaxing of Bamboo Flour. To dewax the samples, weigh approximately 200.0 g

of bamboo flour and wrap them to filter paper. Afterward, prepare 2800 mL of 2:1 v/v
Cyclohexane-Ethanol solution and pour it into the round-bottom flask and place the wrapped
bamboo sample into the macro-soxhlet extractor. Furthermore, the macro-soxhlet extractor
was placed in the thermal heater at a temperature of approximately 250 °C. The extraction
process was continued until the color of the mixture disappeared. Specifically, the extraction
process lasted for at least six (6) hours. Next, the dewaxed bamboo flour was poured into a
beaker and stirred using a glass rod while adding a cyclohexane-ethanol solution.

Figure 3.6 The set-up for dewaxing the B. vulgaris meal flour.

Furthermore, the treated sample was then filtered using a filter cloth while being
washed with hot distilled water. Moreover, it was evenly distributed using a glass rod on a
pan lined with aluminum foil. The dewaxed bamboo sample is then placed in the oven set at
70 °C for at least 24 hours and was kept for the delignification process. Moreover, the pan is
labeled as dewaxed bamboo flour (DBF).

Delignification of Bamboo Flour. The delignification process was conducted by

preparing the solution using 82.3 g of 35 wt% hydrogen peroxide (H2O2) and 106.2 g of 99.8
wt% acetic acid (CH3COOH) in the presence of Titanium (IV) oxide (TiO2; approximately 1.0
g) and pouring it into a round-bottom flask. Furthermore, weigh about two (2) 30.0 g of DBF
and immerse it in the delignification solution. Consequently, place the two (2) flat-bottom
flasks on the heater element and heat it up to 130 °C.

Figure 3.7 The set-up for delignification of B. vulgaris meal flour.

Correspondingly, after two (2) hours of heating, the hot plate was turned off and
cooled to room temperature. Afterward, the treated DBF was filtered using a Buchner flask
and rinsed with deionized water (DI) until the pH level reached 7. As a further matter, the
treated sample was evenly distributed in a Petri dish and subjected to oven-drying (70°C) for
at least 24 hours. Following the drying, the sample was kept in a dark, cool place, ready for
alkaline treatment. Moreover, the treated sample is identified as delignified bamboo flour
(DLBF).

Alkaline Treatment of Bamboo Flour. To remove the hemicelluloses and pectin of

the DLBF, the samples must undergo alkaline treatment. The DLBF was soaked into 50 mL
of 6 wt% sodium hydroxide (6.0 g of NaOH in 100 mL of distilled water) using a 250 mL
beaker. Furthermore, the beaker with the mixture is placed on the hot plate and stirred using
a magnetic stirrer for 120 minutes at 80 °C, and stopped after 480 minutes of stirring.
Afterward, the mixture is cooled to room temperature and filtered using the Buchner flask.
Moreover, the treated bamboo sample is rinsed with deionized water (DI) until it reaches a
pH of 7. Overall, the bamboo sample was then transferred to a Petri dish and air-dried for at
least 36 hours.
 Figure 3.8 The set-up for the alkaline treatment of B. vulgaris meal flour.

3.4 Production of Furanic Bio-oil

Prepare and weigh nine (3) 5.0 g of isolated cellulose and 5.0 g of monohydrate or
anhydrous citric acid and pour them into a large test tube, where they are mixed using a
glass rod. Furthermore, the beaker with the mixture is placed in a hot oil bath and heated at
152°C to 155°C. Specifically, the oil used in the experiment was virgin coconut oil.

The mixture was subjected to various reaction times to measure and determine the
yield of bio-oil at the given time. Particularly, the retention times for the experiment are 120
minutes, 180 minutes, and 240 minutes, and each of the retention times has three (3)
replicates. A total of nine replications are needed for the setup. Furthermore, at the end of
every reaction, after cooling the mixture, 60 mL of acetone is added and the suspended
particles are filtered using a sintered glass connected to an Erlenmeyer flask. Additionally,
another 60 mL is used to wash the citrated cellulose. The collected liquid phase is reduced
with the use of a rotary evaporator set at 65°C. This was done to remove any traces of
acetone and give bio-oil in the form of a brown viscous liquid. In addition, the esterification
process will also produce citrated cellulose as a co-product and it will also be subjected to
different testing conditions for characterization. The setup for the experiment can be seen in
Figure 3.9.
 Figure 3.9 The experimental set-up for the production of furanic bio-oil: (a) weighing of
cellulose and citric acid; (b) cooking of the mixture; (c) reduction of acetone through rotary
evaporator; and (d) extracted furanic bio-oil.

3.5 Physical Characterization of furanic bio-oil

Physical Characterization of furanic bio-oil

Copper Corrosion Test. The produced furanic bio-oils were subjected to determine
their corrosiveness under the specific time and temperature. The test method followed the
ASTM D130 by immersing the polished copper strip into a 100 mL furanic bio-oil and heating
it up to 50°C for about 3 hours. Afterward, the strip of copper is removed and washed, and
the appearance of color and tarnish of the copper strip is assessed based on the ASTM
Copper Strip Corrosion Standard (see Table 3.0).

Table 3.0 The Copper Strip Classification for Petroleum Products.

Classification Designation Description

Freshly Polished Strip

1 Slight tarnish a. light orange, almost the

same as freshly polished
strip
b. dark orange
 2 Moderate tarnish a. claret red

… b. lavender

… c. multicolored with lavender

blue or silver, or both,
overlaid on claret red

… d. silvery

… e. brassy or gold

3 Dark tarnish a. magenta overcast on brassy

strip

… b. multicolored with red and

green showing (peacock),
but no gray

4 corrosion a. transparent black, dark gray

or brown with peacock green
barely showing

… b. graphite or lusterless black

… c. glossy or jet black

Source: ASTM D130 (2019)

Elemental Analysis. The produced furanic bio-oil was analyzed for its elemental
compositions. In the case of carbon, hydrogen, and nitrogen content, 100 mL of furanic
bio-oil undergoes the combustion method using the standards provided by the Standards
and Testing Division (STD) of the Industrial Technology Institute-Department of Science and
Technology (ITDI-DOST). As for the total sulfur content, 250 mL of furanic bio-oil undergoes
monochromatic, wavelength-dispersive X-ray fluorescence (MWDXRF) spectroscopy
following the ASTM D7039.

Kinematic Viscosity. The viscosity value of the produced furanic bio-oil was
determined following the ASTM D445 provided by the STD of ITDI-DOST. In the case of
furanic bio-oil, 200 mL of sample was flown under gravity through the capillary of a calibrated
viscometer under a reproducible driving head at 40°C. The determined value of kinematic
viscosity was the product of the measured flow time and the calibration constant of the
viscometer.

Specific Gravity. The specific gravity of the produced furanic bio-oil was measured
following the ASTM D1298 provided by the STD of ITDI-DOST. A 500 mL sample (furanic
bio-oil) is brought to a specified temperature, which is 15°C and the test portion is
transferred to a hydrometer cylinder that has been brought to the same temperature. The
suitable hydrometer and thermometer are lowered into the testing portion and allowed to
settle. Once the temperature equilibrium is reached, the hydrometer scale is read, and the
temperature of the test portion is taken. Moreover, the observed hydrometer reading is
corrected for the meniscus effect.

pH value. The pH value of the produced furanic bio-oil was measured using a pH
probe with a digital meter (insert the brand of the pH meter), and the calibrated temperature
was recorded at 29°C.

Total Acid Number. The acid number of the produced furanic bio-oil was determined
following the ASTM D974 provided by the STD of the ITDI-DOST. A 200 mL of furanic bio-oil
was dissolved in a mixture of toluene and isopropyl alcohol, which contains a small amount
of water. The resulting single-phase solution was titrated at room temperature with a
standard alcoholic base or alcoholic acid solution, respectively, and the endpoint is indicated
by the color change of the added p-naphtholbenzein solution. As for the determination of the
strong acid number, a separate portion of the produced furanic bio-oil is extracted with hot
water and the aqueous extract is titrated with potassium hydroxide solution, through the use
of methyl orange as an indicator.

Heating Value. The heating value of produced furanic bio-oil was measured through
the application of ASTM D240 provided by the STD of the ITDI-DOST. About 100 mL of
furanic bio-oil was burned in an oxygen bomb calorimeter under controlled conditions. The
combustion for heating is computed from temperature observations before, during, and after
combustion, with proper allowance for thermochemical and heat transfer corrections.

Chemical Characterization of furanic bio-oil

Fourier Transform Infrared Spectroscopy (FTIR) Analysis. The functional groups

of the produced furanic bio-oil using the Perkin Elmer FT-IR Spectrometer Frontier. The
absorption frequency spectra range from 4000 cm-1 to 600 cm-1, while the number of scans is
20. As for the identification of the identified peaks, the reference book from Prestch et al.
(2009) was used.

Gas Chromatography/Mass Spectrometry (GCMS) Analysis. The chemical

composition and the relative composition of the identified compounds in the produced furanic
bio-oil were analyzed by GC-MS Agilent 8890 GC system coupled to a 5977B Mass
Selective Detector. Gas chromatography was performed using an HP-5MS column (30 m ✕
0.250 mm ✕ 0.25 µm film thickness. Helium gas (99.99%) was used as the carrier gas,
having a constant flow rate of 1 mL/min. As for the oven temperature, it was programmed
from 35°C to 300°C at a heating rate of 25°C/min from 35°C to 125°C, and 7°C/min from
125°C to 300°C. The parameters of mass spectrometry were conducted through the
following operational conditions: MS Ionization mode of 70 eV, acquisition mode through
scanning, and mass range of 30 amu to 500 amu. The Agilent MassHunter Qualitative
Analysis 10.00 was used to process the data and the NIST MS Search 2.3 database was
used for the identification of the peaks in the chromatogram.
 4. RESULTS AND FINDINGS

4.1 Proximate Chemical Analysis

Conducting proximate chemical analysis of biomass indicates their composition

concerning moisture content, volatile matters, ash content, and fixed carbon (Kamran, 2023).
Furthermore, the proximate chemical analysis of biomass specifies the percentage of the
actual material that burns during the process. According to Nunes et al. (2018), the
percentage of gaseous state, solid state, and inorganic wastes can be determined when
executing the proximate analysis. Therefore, the characterization of feedstock composition is
necessary to reliably predict its behavior as a biofuel (Garcia et al., 2013).

In the case of B. vulgaris meal flour, the moisture content, ash content, organic
extractives (cyclohexane-ethanol), hot water extractives, lignin content, holocellulose
content, and alpha-cellulose content were determined and calculated. Furthermore, the
summary of the proximate chemical analysis of B. vulgaris is presented in the table below
(see Table 4.0).

Table 4.0 The proximate chemical composition of Kawayan Kiling (B. vulgaris).

Chemical Composition Average Values (%)

Moisture Content (%) 12.9828 ± 0.22

Ash Content (%) 4.6729 ± 0.02

Organic Extractives (%) 2.5683 ± 0.04

Hot Water Extractives (%) 3.9867 ± 0.08

Lignin Content (%) 28.8534 ± 0.17

Holocellulose Content (%) 78.8417 ± 0.52

Alpha-Cellulose Content (%) 72.8297 ± 0.25

Moisture Content of Bambusa vulgaris

In the determination of moisture content (%MC), the gravimetric method was applied
to acquire the values per replicate and the average value. The samples were subjected to
oven-drying for two (2) while measuring the mass of each replicate per day to determine if
the weight of the three (3) samples are constant. Furthermore, after two (2) days of drying,
the mass of the three (3) samples became constant from 2.00 g (initial weight) to 1.77 g
(oven-dried weight), acquiring a moisture content of 12.7281% to 13.4153% and average
moisture content of 12.9828%. In comparison with the paper of Razal (2014), the obtained
moisture content for B. vulgaris was lower than the obtained %MC, having a value of
8.672%. On the other hand, in the study conducted by Gomes-Neto (2021) on the physical
and mechanical properties of B. vulgaris, the obtained an average moisture content for B.
vulgaris of 12.21%, which is partially close to the obtained value.

Figure 4.0 The B. vulgaris flour after subjecting to oven-drying for two (2) days.

Furthermore, Wang et al. (2019) reported that the moisture content of bamboo
species varies from 10% to 15% in tropical countries. Based on the variation manifested by
the obtained values as compared to other studies, it should be noted that the %MC of a
hygroscopic material, for instance, B. vulgaris flour, can be different from sample to sample
since moisture content depends on the humidity and the environment where the samples
came from. According to Williams et al. (2017), the innate variability between the samples of
the same species, for instance, B. vulgaris, can be attributed to growth characteristics,
weather conditions, and humidity in the area. Aside from the reasons mentioned above why
there is variation in %MC of B. vulgaris, Sreeja-Devi (2016) argues that variations in
moisture content can also be related to the portion where samples are collected, such as the
top, middle, and bottom. For instance, Gomes-Neto et al. (2021) supported the claim of
Sreeja-Devi (2016) as the obtained %MC for different parts of B. vulgaris differ from one
another, specifically, the middle part of the bamboo pole obtained the highest %MC of
12.61%, followed by the base with 12.48%, and lastly, the top portion of the pole obtained
the lowest %MC of 11.53%.

Ash Content of Bambusa vulgaris

 In terms of the ash content of B. vulgaris, the average value obtained from the
proximate analysis was 4.6729% since the acquired mass of ash after the combustion (at
600 ℃) ranges from 0.0465 g to 0.0472 g. Furthermore, the % ash content of B. vulgaris
ranges from 4.6467% up to 4.7158% (see Figure 4.1). However, in comparison with the
findings of Jara et al. (2018), the ash content of B. vulgaris was quite high as compared to
the obtained values. Based on the study, the obtained ash varies depending on the height of
the bamboo pole and the season where it is collected. For instance, higher concentrations of
ash content were identified in the B. vulgaris collected during the end of the rainy season
than in the bamboo collected before the onset of rainy season. For the ash content of B.
vulagris collected during the onset of the rainy season, the % ash ranges from 9.06% to
10.86%, having the highest value from the bottom part of the bamboo. On the other hand,
the amount of ash obtained from the samples collected at the end of the rainy season varies
from 10.19% to 11.62%, with the highest amount concentrated in the bottom part. On the
other hand, in the study of Espiloy (1996), the obtained ash content for B. vulgaris is 2.4%,
while in the paper of Razal (2014), the obtained organic extractives is 4.691%, which is
closely related to the obtained values.

Figure 4.1 The obtained ash content from B. vulgaris after subjecting to combustion for 30
minutes.

The effect of harvesting time affects the accumulation of minerals and nutrients in
bamboo. Specifically, it can be attributed that at the end of the rainy season, the amount of
water is abundant compared to the amount it has before the onset of the rainy season.
Consequently, the abundance of water leads to the accumulation of greater mineral content,
such as calcium, potassium, sodium, magnesium, manganese, and phosphorus, which
constitute the chemical composition of ash (Babayemi et al., 2010; Jara et al., 2018).
 Moreover, the variation in the obtained value for ash content to other studies can be
attributed to the location, time of collection, and the condition of the environment.
Garcia-Maraver et al. (2015) argued that the chemical composition of biomass varies within
the same species due to the existing conditions of the environment where it is collected, and
the weather conditions during the time of collection. Additionally, the conditions of the soil
may also affect the ash content of the sample since the availability of inorganic nutrients
depends on the quality of the soil in the area (Siddique, 2007).

Organic Extractives Content of Bambusa vulgaris

In the case of the organic extractive presence in B. vulgaris, the content ranges from
0.7050% to 0.8400%, with an average of 0.7667% (see Figure 4.2). Specifically, the first
replicate obtained an amount of 0.7550%, while the second and third replicates obtained an
amount of 0.8400% and 0.7050%, respectively. However, in comparison to the study
conducted by Jara et al. (2018), the extracts extracted were 5-9 times higher than the
obtained values from the meal of B. vulagris, varying from 9.16%, 7.31%, and 6.41% for the
samples obtained before the onset of the rainy season, while the % Organic extractives for
B. vulgaris obtained after the rainy season had a value of 5.71%, 7.21%, and 5.28%.
Meanwhile, in the study conducted by Razal (2014) for proximate chemical analysis of
selected Philippine bamboo species, the % Organic solvents obtained for B. vulgaris is
8.958%, while Espiloy (1996) acquired an amount of 4.1%.

Furthermore, the low organic extractive content of B. vulgaris indicates that the
bamboo culm had fewer organic substances, such as phenolics including flavonoids and
other organic matter. According to Sulaiman et al. (2016), the organic extractives of B.
vulgaris range from 0% to 5%, depending on the conditions of species, age, climate, and
harvesting time. Moreover, the chemical composition of cell wall structures influences
organic extractives since bamboo fibers are suspended in a soft matrix mostly consisting of
lignin and hemicelluloses. Additionally, Ma et al. (2014) reported that most of the substances
found in B. vulgaris are more soluble in water than the organic solvents, and these
substances are resins, fatty acids, terpenoid compounds, and alcohols.
Figure 4.2 The Organic Extractives (Cyclohexane-Ethanol) of B. vulgaris were obtained from
Soxhlet Extraction. (a) Replicate; (b) Replicate 2; (c) Replicate 3.

Meanwhile, when it comes to the color obtained from the extraction of organic
extractives (see Figure 4.2) the appearance of each replicate varies from each other. In
replicate 1, the obtained extractives appear to be darker compared to two (2) other samples.
Additionally, there is a layer of water in the round bottom flask making it immiscible to each
other. As for replicate 2, the extracted organic extractives appear to be cloudy but lighter
yellow in color as compared to replicate 1 and replicate 3. In the case of replicate 3, there is
also a formation of water in the round bottom flask making it immiscible to each other;
however, compared to replicate 1, replicate 3 appears to be a little bit lighter (yellow) in color.
Moreover, the extractives obtained from the process are responsible for the colors of the raw
material from the plant (Hartono et al., 2022). In the case of Kawayan Kiling, the color may
elucidate dark yellow to light yellow color. However, the degree of color may vary per
replicate depending on the samples collected.

In the case of the presence of water in the acquired extractives, it can be attributed to
the soxhlet extraction process itself. According to Lao et al. (1996), the technique of using
soxhlet extraction has some drawbacks due to restrictions in solvent selectivity. For instance,
the extraction process requires the boiling point of the solvent being used, and the samples
are boiled for a long period of time, for instance, a minimum of four (4) hours. Consequently,
the longer the sample is boiled, the possibility of the thermal decomposition of samples can
occur, leading to contamination of the obtained organic extractives with large amounts of
solvent impurities (Lao et al., 1996; Shu et al., 2000). Moreover, the presence of mold inside
the condenser due to aging can be considered another source of contamination/inaccuracy
in the results; hence, the organic extractives obtained are lower compared to other literature.
 Moreover, the oven-dried organic extractives of B. vulgaris manifest darker yellow in
color (see Figure 4.3). Replicate 1 has a darker color as compared to the two (2) oven-dried
extractives (see Figure 4.3a). As for Replicate 2, it is lighter in color compared to Replicate 1
and it obtained the highest amount of organic extractives (see Figure 4.3b). In the case of
Replicate 3, the appearance of its extractives is the lightest of three (3) samples and
obtained the lowest amount of organic extractives (see Figure 4.3c).

Figure 4.3 The oven-dried Organic Extractives of B. vulgaris: (a) Replicate 1; (b) Replicate
2; (c) Replicate 3.

Hot Water Extractive Content of Bambusa vulgaris

The obtained hot water extract (%) from B. vulgaris for the three (3) replicates (R1,
R2, R3) is 3.9650%, 3.8600%, and 4.1350%, respectively, while the average value for the
replicates is 3.9867%. In comparison in the study of Espiloy (1996), the amount of obtained
hot water extractives was 4.1%, which is slightly higher than the obtained average value. On
the other hand, in the proximate analysis conducted by Razal (2014), the hot water
extractives content obtained is almost similar to the content acquired, having a value of
3.655%. Similarly, Lin et al. (2013) gain almost similar results for hot water extractives, with a
% content of 3.61 for B.dolichoclada.

Furthermore, Hossain et al. (2022) reiterated that Bambusa sp, specifically B.

vulgaris is more susceptible to hot water extraction as compared to other solvents, such as
1% NaOH Solubility and Ethanol-Benzene Solubility. Additionally, in the study conducted by
Maulana et al. (2020), it was found that most of hot water extractives obtained from
Bambusa sp, specifically in B. vulgaris contain tannins, gums, low molecular weight
carbohydrates, dyes, and starch. Jara et al. (2018) also stated that water-soluble extractives
of B. vulgaris may contain high amounts of carbohydrates, specifically carbohydrate-rich
fractions, which can be used for the production of bioethanol (Almodares & Hadi, 2009).

In terms of the color of the water extractives, Replicate 1 and Replicate 2 manifest
darker yellow color as compared to Replicate 3 which shows a beige-yellow color (see
Figure 4.4).

Figure 4.4 The Hot Water Extractives of B. vulgaris after the Soxhlet Extraction: (a)
Replicate 1; (b) Replicate 2; and (c) Replicate 3.

Despite having a similar color appearance to Replicates 1 and 2, it was found in the
study that Replicate 3 obtained the highest amount of hot water extractives compared to
Replicates 1 and 2 with a deeper yellow color. In fact, Replicate 2 had the lowest hot water
extractives, while Replicate 1 is almost higher than 0.105% as compared to Replicate 2. The
obtained results from hot water extraction can be correlated with the obtained extractives in
the Cyclohexane-Ethanol. For instance, the highest value among the three (3) replicates in
% Organic Extraction is Replicate 2; therefore, it can be inferred that the possibility of
Replicate 2 having the lowest amount of % Hot Water Extractives is due to the highest
amount of material extracted from nonpolar solvent. Moreover, this trend can be attributed to
the study of Maulana et al. (2020) whereas B. vulgaris has a larger amount of extractives to
hot water solubility as compared to the solubility using organic solvents.

Lignin Content of Bambusa vulgaris

 In determining the lignin content of B. vulgaris, the Klason method was used in the
study. The extractive-free B. vulgaris flour was treated with 72% sulfuric acid (H2SO4) that
undergoes hydrolysis and condensation reactions. Furthermore, based on the obtained
values, the average lignin content of B. vulgaris (see Figure 4.5) is 28.8534%, while each
replicate acquired a value of 28.7002% (R1), 29.1803% (R2), and 28.6716% (R3). In
comparison with the study of Razal (2014), the obtained % lignin was slightly higher than the
obtained values at 30.463%. In contrast to the results obtained by Espiloy (1996), the
amount of % lignin was slightly lower than the obtained values at 26.98%. On the other
hand, in the study conducted by Jara et al. (2018), the lignin content varies depending on the
time of harvesting of B. vulgaris. For instance, B. vulgaris harvested during the onset of the
rainy season have more lignin content, with an average value of 18.51%, compared to B.
vulgaris harvested at the end of the rainy season, with an average value of 13.7%.

Figure 4.5 The obtained Klason lignin from B. vulgaris: (a) Replicate 1;
(b) Replicate 2; and (c) Replicate 3.

The variation in lignin content can be attributed to the maturity of the bamboo
(Murphy & Alvin, 1997). This can be proved in the study of Jara et al. (2018) since there is
an increasing trend with the amounts of lignin as the bamboo pole elongated. In fact, Jara et
al. (2018) stated that within the 30 cm and 60 cm of B. vulgaris, the amount of lignin is less
than compared to the 90-cm mark. Furthermore, Sulaiman et al. (2016) supported the claim
that the top portion of B. vulgaris contains more lignin due to its anatomical structures.
Specifically, the top portion has a thicker middle lamella layer and a thicker cell wall, and
according to Panshin and Zeeuw (1980), the highest concentration of lignin can be found in
the middle lamella of the cell walls.

Other studies suggest that high lignin content in bamboo can be accounted for by the
presence of non-lignin components, such as proteins, which can interfere with the
determination of Klason lignin (Jara et al., 2018). The study of Han and Rowell (1997)
showed that non-wood fibers, for instance, bamboo, may contain high amounts of protein.
Consequently, as hydrolysis and condensation occur, the possibility of high Klason lignin can
be achieved.

Holocellulose Content of Bambusa vulgaris

The amount of holocellulose obtained from the extraction process for each replicate
is 78.3428% (R1), 79.8838% (R2), and 78.2984% (R3), while the average holocellulose
content of B. vulgaris is 78.8417%. Furthermore, the acquired amounts of holocellulose can
be seen in the figure below (see Figure 4.6). However, in the paper of Razal (2014), the
amount of holocellulose was slightly lower than obtained values at 67.113% As for Espiloy
(1996), the amount of holocellulose of Philippine-grown B. vulgaris was lower than that of
Razal (2014) and the conducted study at 66.5%. Moreover, Jara et al. (2018) reported that
the amount of holocellulose obtained from the proximate analysis varied from 36.7% to
49.9%.

Figure 4.6 The amount of holocellulose obtained from the

extractive-free meal flour of B. vulgaris
 Holocellulose refers to the total fractional polysaccharides made up of alpha-cellulose
and hemicellulose (Maulana et al., 2020). The variation in the holocellulose can be attributed
to the age of bamboo and the portion where it is collected. According to Sulaiman et al.
(2016), the anatomical structure of the top portion of young B vulgaris influences the amount
of holocellulose due to the thickening of the S1 layer from the secondary wall. As a result, the
vascular bundles have rich sugar content which contributes to the amount of cellulose and
hemicellulose in the cell wall.

Alpha-Cellulose Content of Bambusa vulgaris

Alpha-cellulose pertains to cellulose with a degree of polymerization above 200, and

this chemical composition cannot be dissolved in strong bases solution due to strong
intermolecular bonds (Maulana et al., 2020). Furthermore, the amount of alpha-cellulose
(see Figure 4.7) obtained from the holocellulose for each replicate is 73.3018% (R1),
72.7437% (R2), and 72.4436% (R3), with an average value of 72.8297%.

Figure 4.7 The obtained alpha-cellulose from B. vulgaris: (a) Alkaline Treatment of
holocellulose of B. vulgaris; (b) the obtained alpha-cellulose.

However, in comparison to the study of Jara et al. (2018), the amount of

alpha-cellulose acquired is relatively lower than the obtained value at 14.25% to 18.52% for
B. vulgaris harvested at the onset of the rainy season. Meanwhile, the same trend was
observed for B. vulgaris harvested at the end of the rainy season, having a value ranging
from 28.75% to 29.63%. On the other hand, in the paper of Razal (2014), the obtained value
for alpha-cellulose is slightly higher than the acquired value at 67.113%. Furthermore,
Sulaiman et al. (2016) conducted a study on the chemical composition of young and mature
B. vulgaris as well as its cell wall structure, and it was found that mature B. vulgaris obtained
a higher amount of alpha-cellulose compared to young shoots. The value ranges from
52.02% to 58.50%, while the young bamboo pole ranges from 46.43% to 52.93%.

Furthermore, the difference in values can be accounted for by the anatomical

structure of B. vulgaris. According to Sulaiman et al. (2016), the middle portion of a mature
B. vulgaris is composed of larger and longer fiber size and the outer portion of the
cross-section exhibited a complex vascular bundle structure as compared to the inner
portion. Moreover, Widja and Risyad (1985) expound that the fiber size is greater in the
middle portion as compared to the top and bottom, while the outer part of the culm had
longer fibers than the inner portion, resulting in high amounts of alpha-cellulose.

4.2 Yield and Reaction Mechanism of Furanic Bio-oil

Yield of furanic bio-oil

The production of Furanic bio-oil was subjected to three (3) different time conditions,
such as after two (2), three (3), and four (4) hours in order to determine its effect on the
possible yield of Furanic bio-oil. Furthermore, the effect of time retention has a significant
effect on the acquired yield for bio-oil (see Table 4.1). On the other hand, the weight
equivalents for Citric acid (CA) remain the same.

Table 4.1 The summary of the acquired yield of Furanic Bio-oil under the three (3) different
time retention conditions.

Time (min) Average Furanic Bio-oil Yield (%)

120 minutes 59.2756 ± 1.77

180 minutes 88.5892 ± 4.36

240 minutes 49.9554 ± 0.0049

The acquired average furanic bio-oil yield for each time retention is 59.2756% after
two hours, 88.5892% after three hours, and 49.9554% after four hours. Furthermore, it can
be seen that after three hours of cooking in the hot bath, the yield of furanic bio-oil is at its
peak based on the computed average yield per time retention. Additionally, it can be noted
that the average yield of furanic bio-oil after four hours of cooking declined from the previous
88.5892% to 49.554%. Moreover, the overall trend for the yield of furanic bio-oil is similar to
that of a bell-shaped normal curve (see Figure 4.8), since after 2 hours of cooking the trend
increase until it reaches its peak at the 3-hour mark time, and after that, the trend went down
after 4 hours of cooking time.
 Figure 4.8 The trend in the yield of furanic bio-oil in relation to time retention.

The trend in the yield of bio-oil can be attributed to the reaction mechanism that happened in
the cooking of cellulose with citric acid in solvent-free conditions. According to Romeo et al.
(2020), the yield and composition of furanic bio-oil are strongly influenced by time retention.
As a matter of fact, during the process of cooking the cellulose and citric acid from two hours
up to three hours, the bio-oil composition resulted in rich furan compounds and carboxylic
acids (Romeo et al., 2020). Therefore, the yield of furanic bio-oil is high within the time frame
due to the presence of organic compounds, such as furans, carboxylic acids, and others.

Furthermore, with the declination of yield after more than three hours of cooking,
significant oxidation occurs within the furanic compounds. Additionally, Romeo et al. (2020)
reiterated that addition to the retention time increases the oxidation and volatility of the
furanic compounds, leading to uncontrolled decomposition of furan compounds and other
organic compounds present in the bio-oil. Moreover, using the melting point of citric acid and
cooking the mixture for three hours, Romeo et al. (2020) reported that after this time frame,
most of the cellulose is depolymerized in a mixture of compounds extracted with the use of
acetone, producing a dark brown furanic bio-oil. Additionally, after the 3-hour benchmark
time, 80% of the cellulose is hydrolyzed to furanic bio-oil; hence, the highest yield occurs in
this time retention (Romero et al., 2020; Kassanov et al., 2022).

Reaction Mechanism of furanic bio-oil

To elucidate the mechanism of producing and extracting furanic bio-oil (see Figure
4.9), the principles of hydrolysis and esterification were applied in the process. The process
of cellulose hydrolysis is due to the functionalities of citric acid interacting with the glycosidic
bonds of the cellulose chains (see Figure 4.9a) and the oxygen in the pyranose rings (see
Figure 4.9b) (Romeo et al., 2020).
 Figure 4.9 The interactions of citric acid in the cellulose: (a) in glycosidic bonds; (b) in the
oxygen of pyranose.
Source: Romeo et al. (2020)

Specifically, the isolated cellulose is depolymerized to glucose units (see Figure

4.10a) through the help of traces of water and the acids present in the carboxylic groups of
citric acid. Furthermore, the traces of water present in the reaction is due to the open system
conditions of the set-up. Once the glucose is formed, it reduces quickly due to the
open-system condition mechanism by losing three (3) molecules of water, leading to the
production of furan-rich bio-oil (see Figure 4.10b).

Moreover, once the furan-rich compound, for instance, 5-hydroxymethylfurfural, is

produced, this compound can initiate a sequence of oxidation reactions that produce other
furan compounds (see Figures 4.10c, 4.10d, and 4.10e). Furthermore, the moieties
formation in carboxylic acids during the oxidation to furan compounds is confirmed by
measuring the pH value of the compounds. According to Romeo et al. (2020), the pH value
ranges from 4.2 to 4.4 after 30 minutes of reaction, and 3.0 to 3.2 after an overnight reaction.

Figure 4.10 The hydrolysis of cellulose catalyzed by citric acid at 155 °C and under
open-system conditions leads to furanic bio-oil production
Source: Romeo et al. (2020).
4.3 Physical Properties of Furanic Bio-oil

The physical characterization of furanic bio-oil was utilized to determine the basic
properties it exhibited under the specific conditions of two hours, three hours, and four hours
using the melting point temperature of Citric acid, which is 155 °C. Furthermore, Table 4.2
summarizes the physical characterization of the produced furanic bio-oil, and compares it to
other bio-oil produced using the same genus (Bambusa sp) of the material used and other
forest-based biomass materials.

Table 4.2 Summary of physical characterization of furanic bio-oil under three (3) different
time conditions.

Furanic Bio-oil
Parameters, Unit
2 hours 3 hours 4 hours

S, wt. % * 0.032 *

Kinematic Viscosity at 0.367 1.03 0.368

40°C, mm2/s

Specific Gravity @ 15°C 0.794 0.925 0.794

Copper Corrosion Test @ No. 1a** No. 1a** No. 1a**

50°C for 3 hours

pH value 2.75 2.753 2.76

Water Content * Not Detected *

*Some of the test analyses are still in the process, such as CHN, Heating Value, Total Acid
Number, Sulfur content for 2 hours and 4 hours and Water Content for 2 hours and 4 hours;
hence, the presented parameters in the table are the available ones.
**Slightly tarnish; light orange, almost the same as freshly polished strip

The kinematic viscosity of three-hour B. vulgaris-derived furanic bio-oil is higher than

that of the two-hour and four-hour derived furanic bio-oil. Based on the achieved value for
viscosities, the three-hour extracted furanic bio-oil has a value of 1.03 mm2/s, while the
two-hour and four-hour extracted furanic bio-oil had a value of 0.367 mm2/s and 0.368
mm2/s, respectively. Furthermore, the four-hour extracted oil is higher by 0.001 value as
compared to the two-hour extracted oil. Moreover, the variations in the obtained kinematic
viscosity can be attributed to the cooking of the furanic bio-oil since it influences the
chemical composition of the bio-oil and the yield acquired.

Additionally, the low amount in viscosity for the furanic bio-oil as compared to other
bio-oil produced can be ascertained by the method used and the presence of water
(Broumand et al., 2020). Furthermore, Sondakh et al. (2019) reported that viscosity is the
ability of the liquid to resist when flowing in a particular direction; therefore, if the viscosity is
higher, the flow resistance will also be higher. Furthermore, since the achieved kinematic
viscosity for furanic bio-oil is lower compared to other bio-oils produced, then the usage of
furan-based bio-oil would be efficient and environmentally friendly because lower viscosity
may improve the economy of fuel by reducing greenhouse gas emissions and would have a
better application (White, 2022; Sondakh et al., 2019).

In terms of the specific gravity, the acquired value for the three-hour furanic bio-oil is
0.925, or in density, the equivalence would be 925 kg/m3. As for the two-hour furanic bio-oil
and four-hour furanic bio-oil, the same values were obtained for specific gravity at 0.794, or
794 kg/m3 in density. It could be indicated that the two-hour and four-hour furanic bio-oils
had lower values as compared to the optimized furanic bio-oil. Meanwhile, in contrast to the
commercially available diesel produced in the market, the achieved value for the optimized
furanic bio-oil is comparatively higher. According to Willimas et al. (2021), the specific gravity
of the commercial automotive no. 2 diesel ranges from 0.820 to 0.860; hence, the three-hour
furanic bio-oil has a higher energy content as compared to the conventional diesel, and the
two-hour and four-hour produced furanic bio-oil. Moreover, the specific gravity indicates the
energy value of the bio-oil, and the higher the specific gravity, the higher the energy value of
the bio-oil (Ahmad et al., 2022).

As for the copper corrosion test, the achieved designation for the optimized furanic
bio-oil was No. 1a, which means it causes a slight tarnish to the metal and had an
appearance of light orange which is almost the same as a freshly polished strip. Moreover,
the extracted furanic bio-oil from B. vulgaris is not corrosive as compared to other biodiesel
produced in the market. In the study of Milano et al. (2021), biofuels can have drawbacks as
these products can cause metallic corrosion in some parts of the engine, such as fuel
pumps, filter lines, injectors, etc. Moreover, in the study conducted by Yesilyurt et al. (2022),
the corrosion of metal can be due to sulfur content, the amount of water present, and the
degree of acidity. Therefore, the necessary and standard classification of biofuel in terms of
corrosion value should be in class 1 (Jung et al., 2006), which resonates with the obtained
classification in the study.

The pH value of the furan-based bio-oil can be influenced by various factors, such as
the type of biomass used and the type of solvent used to extract the bio-oil (Ahmad et al.,
2022). Furthermore, due to the presence of organic acids, such as carboxylic acid and acetic
acid, the pH value obtained by the optimized furanic bio-oil is 2.753 ± 0.0033. Meanwhile,
the two-hour and four-hour produced furanic bio-oil obtained a pH value of 2.75 and 2.76,
respectively. Furthermore, due to the presence of organic acids, such as carboxylic acid and
acetic acid, makes the bio-oil acidic in nature. However, Lian et al. (2017) reiterated that the
acidity of bio-oil can be reduced through the conversion of acids into esters through the
process of esterification.

In terms of the sulfur content, based on the study of Ahmad et al. (2022) and Lu et al.
(2008), it is usually low in concentration due to the nature of the biomass used. Therefore,
the acquired sulfur content for the three-hour produced furanic bio-oil is 0.032%. Moreover, a
lower concentration of sulfur imposes a positive trait since the amount of sulfur in bio-oil
indicates the possible amount of hazardous sulfur dioxide during the combustion process
(Ahmad et al., 2022; Lu et al., 2008; Yesilyurt et al., 2019).

Water content in bio-oil can be attributed to the moisture of the biomass used and the
method applied during the process of extraction (Ahmad et al., 2022). Furthermore, the
presence of water in bio-oil or biofuel can form a separate layer of the aqueous phase and
organic phase, which causes problems in the application of bio-oil in the industry (Fregolente
et al., 2012). The water content achieved in the study was 0%, or not detected due to the
nature of the furan-based bio-oil. As a further matter, the 0% water content can be attributed
to the method used in the extraction of bio-oil. The solvent-free condition application can be
the reason why furanic bio-oil is negligible in terms of water content. Moreover, He et al.
(2007) reported that higher moisture content/water content in biofuel or biodiesel can impose
severe problems, such as the accumulation and growth of microorganisms in fuel tanks and
transportation equipment (He et al., 2007; Fregolente et al., 2012); Ahmad et al., 2022).
Overall, the commercial automotive diesel No. 2 had 0.008% of water content (Williams et
al., 2021).

4.4 Chemical Properties of Furanic Bio-oil

The chemical characterization of the produced furan-based bio-oil is necessary to

conduct in order to determine the chemical composition and the functional groups present in
the product. According to Zhang et al. (2013), the chemical characterization of bio-oil is
essential for the identification of important chemicals, which can be the basis for the
production and synthesis of biofuels.

Fourier Transform Infrared Spectroscopy (FTIR) Analysis

The FTIR Spectroscopy analysis of furan-based bio-oil is summarized in the table

below (see Table 4.3). FTIR analysis, according to Lievens et al. (2013), is an analytical
technique used in the characterization of functional groups in the bio-oil.

Table 4.3 The functional groups found in the FTIR of furanic bio-oil.

Frequencies (cm-1) Structure/ Bonds*

Compound
Standard Type
Group 2 hours 3 hours 4 hours
Frequencies

3550-3000 3425.00 3444.03 3448.80 Carboxylic COO-H

Acid Stretch

Carboxylic COO-H
3000-2840 2928.57 2928.57 2929.75 Acid Stretch

Alkane C-H Stretch

2840-2500 2603.57 2603.57 2603.57 COO-H

Stretch

1763.14 1764.31 1764.58

1800-1650 C=O Stretch
1705.61 1699.22 1703.55
Carboxylic
1416.80 1417.19 1418.86 Acid
OC-OH
1361.68 1363.99 1361.74 Stretch/
1440-1210 C-OH Bend
 1272.35 1274.14 1274.14

1221.07 1227.77 1223.57

1177.83 1188.53 1177.83

C-H Skeletal
1210-960 1094.01 1092.70 1092.48 Alkane Vibration
1024.45 1028.02 1026.24

960-880 908.10 910.65 910.73 Carboxylic OC-OH

Acid Bend

770-720 733.27 734.20 733.96 Alkane C-H Skeletal

Vibration
* Reference: Pretsch, E., et al. (2009). Structure Determination of Organic Compounds, 4th
Ed., Springer - Verlag Berlin Heidelberg.

The strong frequency peaks of furan-based bio-oil between 3550 cm-1 and 3000 cm-1
denote the presence of carboxylic acid due to the presence of COO-H Stretching. On the
other hand, the frequenct range of 3000 cm-1 and 2840 cm-1 specify the possibility of having
carboxylic acid and alkane compounds in the produced furanic bio-oil since there are
COO-H stretch and C-H stretch. Furthermore, the frequencies that ranges from 2840 cm-1
and 2500 cm-1, 1800 cm-1 and 1650 cm-1, and 1440 cm-1 and 1210 cm-1 show the possible
presence of carboxylic acid since the identified bonds are COO-H stretch, C=O stretcg, and
OC-OH stretch/C-OH stretch. The 1210 cm-1 and 960 cm-1 mark the presence of alkane due
to their strong and sharp appearance and with the presence of C-H skeletal vibration. As for
the frequency peaks between 960 cm-1 and 880 cm-1, the identified organic compound is
carboxylic acid since there are OC-OH bend determined in the peaks. Moreover, the peaks
recognixed within the 770 cm-1 and 720 cm-1 pertain to the presence of C-H skeletal
vibration, signifying the presence of alkane compounds.

Gas Chromatography-Mass Spectrometry (GCMS) Analysis

The quantification (relative composition) of chemical compounds present in the bio-oil

was identified using GCMS analysis as presented in Table 4.4. A number of organic
compounds are listed in the table below. Furthermore, the total identified compounds in the
furan-based bio-oil are 56, which means that the liquid oil contains a complex mixture of
compounds with multifunctional groups (Lin et al., 2013). However, only the first 10 chemical
compounds with detected highest amounts were considered and expressed in the table,
alongside their corresponding % relative amount.

Table 4.4 The 10 chemical compounds with the highest amounts identified in furanic bio-oil.

No. Chemical Compound Relative

Composition
(%)

1 3-methyl-2,5-furandione 21.58
 2 3-methylene-1-oxaspiro(3.5)nonan-2-one 16.16

3 Butyl citrate 9.34

4 8a-methylhexahydro-1,8(2H,5H)-naphthalenedione 6.37

5 2-methyl-4,5-bis(hydroxymethyl)pyridine 4.15

6 dihydro-3-methylene-2,5-furandione 3.64

7 Dodecanoic acid 2.95

8 ɑ-(3-methylphenoxy)propanoic acid 2.93

9 2mercaptobenzothiazole 1.84

10 trans-2-(2-pentyl)furan 1.46

Furthermore, the specified functional groups are also identified based on the relative
amounts (see Table 4.5) as it demonstrates in the FTIR spectra, and somehow consistent
with the identified functional groups. In fact, the table containing the organic compounds
shows the relative proportion of the individual-compound functional groups from B. vulgaris.
Additionally, the chemical sum and peak areas in the furanic bio-oil extracted from B.
vulgaris were identified and summarized in Figure 4.12. Moreover, the composition of
furan-based bio-oil was compared to other studies wherein bio-oil was also the subject of
chemical analysis.

Table 4.5 The proportions of individual-compound functional groups of furanic bio-oil based
on the identification from the GCMS analysis.

No. Functional Group/ Organic Compound Relative Composition (%)

1 Acid anhydride 0.32

2 Aldehyde 0.95

3 Alcohol 1.54

4 Alkyl halides 0.55

5 Alkane 0.21

6 Amine 3.87

7 Carboxylic acid 19.26

8 Carbohydrates 2.22

9 Fatty acids 7.50

10 Furans 28.19
 11 Esters 6.44

12 Diazo 0.31

13 Ketone 26.31

14 Sulfhydryl 1.72

15 Sesquiterpenoids 0.59

As a result of the GCMS analysis, there are three (3) organic compounds prevalent in
the produced furanic bio-oil from B. vulgaris. The dominating organic compound was the
furans, having a value of 29.19%. Some of the furans identified in the bio-oil include
3-methyl-2,5-furandione, dihydro-3-methylene-2,5-furandione, 3-methyl-4-
propyl-2,5-furanone, and trans-2-(2-pentyl) furan. Furthermore, the 3-methyl-2,5-furandione
had the highest concentration in the furanic bio-oil, accounting for the 21.58% of the total
compounds identified.

Moreover, furan compounds have many applications in terms of biofuel production.

According to Ahmad et al. (2022), furan is essential for the refining process of petroleum
products. In fact, the dominant amount of furan in the produced bio-oil suggests that this
product can be used as a replacement for conventional fuels, or can be an additive to reduce
the GHGs emission of fuels. In addition, Ahmad et al. (2022) reported that furans are mostly
applied as alternatives for oxygenated fuels, which can be extracted from cellulose or even
from the hemicellulose of biomass. Aside from the alternatives for oxygenated fuels,
furan-rich compounds can be used as additives due to their high volatility as the result of
present oxygen bonds in the compound. As a matter of fact, Abdellatief et al. (2021) stated
that furanic compounds have a promising value as these compounds impose high heating
value, low water solubility, and are excellent in volatility. More importantly, the application of
furan in the petrochemical industry can reduce particulate matter emission much more
efficiently compared to conventional fuels (Ahmad et al., 2022).

The compound present in the second-highest amount is ketone, having a relative

proportion of 26.31%. Ketone is a widely utilized chemical in the industry for being a versatile
compound. According to Torres-Vinces et al. (2020), the probability of using ketones (i.e.,
MEK) as a main ingredient in fuel production is accepted since methyl ethyl ketone (MEK)
has a considerable performance in spark engines as compared to the use of gasoline.

Furthermore, the production of MEK from a renewable resource can be accounted for
as a relief due to the excessive emissions of GHGs through the use of conventional fuels.
Aside from the MEK production, the engineering of Escherichia coli (E.coli) in order to
overproduce saturated and monosaturated methyl ketones has potential applications in the
production of biofuel (Goh et al., 2012). Moreover, the amount of produced and identified
ketones in the study is considerably higher as being the second most abundant organic
compound in the produced furanic bio-oil, having a relative composition of 26.31%.

Other organic compounds present in the furanic bio-oil are carboxylic acids, with total
relative amounts of 19.26%. Furthermore, fatty acids were also identified in the furan-rich
bio-oil, having a relative composition of 7.50%. As for the esters compound, 6.44% were
found to be in the furanic bio-oil. Moreover, the remaining organic compounds are as follows:
Amine (3.87%), Carbohydrates (2.22%), Sulfhydryl (1.72%), Alcohol (1.54%), Aldehyde
(0.95%), Sesquiterpenoids (0.59%), Alkyl halides (0.55 %), Acid anhydride (0.32%), Diazo
(031%), and Alkane (0.21%).

4B. OUTPUTS

Publication

● Draft two (2) journal articles submitted for publication

Patent/Intellectual Property

● Processing of trademark for “Bambu Bio-oil”

Product

● Furanic bio-oil with known properties

● Citrated cellulose from bamboo with known properties

People Service

● Undergraduate Student

4C. OUTCOMES

The development of Bambu-oil and cellulose citrate co-product will help generate
greater value for bamboo planted by farmers in regions where climate favors their growth
and where bamboo growing has become a socially-accepted income-generating economic
activity. This will spur increased demand for bamboo and make available to the bamboo
farmers additional market options for selling their products. The expansion of market
opportunities will mean greater impetus for planting bamboo, with desirable multiple
outcomes such as environmental conservation, forest protection, and livelihood generation.

The study will demonstrate the potential of bio-oil production from bamboo. The study
will serve as the proof of concept and eventually, this will lead to a full-blown research
project. In the long run, it is expected that the technology and/or product that will be
developed be adopted by at least one company and its utility for other applications can be
expanded, explored, and realized.

4D. POTENTIAL IMPACTS (2Is)

Social Impacts

This study aims to make Filipinos more aware of bamboo's utilization, its advantages,
and its potential as a source of value-added products.
Economic Impacts

The study situates itself as part of the plan that is geared towards the alleviation of
the economic status of smallholding farmers. In addition, this project is expected to improve
the competitiveness of the Philippine bamboo market by coming up with new and
environment-friendly products using lignocellulosic materials.

5. LITERATURE CITED

Abdellatief, T. M., Ershov, M., Kapustin, V. N., Abdelkareem, M. A., Kamil, M., & Olabi, A. G.
(2021). Recent trends for introducing promising fuel components to enhance the
anti-knock quality of gasoline: A systematic review. Fuel, 291, 120112.
https://doi.org/10.1016/j.fuel.2020.120112
Abolhosseini, S., Heshmati, A., & Altmann, J. (2014). A Review of Renewable Energy
Supply and Energy Efficiency Technologies (ZA DP No. 8145).
https://docs.iza.org/dp8145.pdf
Ahmad, F., Kalam, M. A., Zhang, Z., & Masjuki, H. H. (2022). Sustainable production of
furan-based oxygenated fuel additives from pentose-rich biomass residues. Energy
Conversion and Management: X, 100222.
https://doi.org/10.1016/j.ecmx.2022.100222
Ahmad, S. F. K., Ali, U. F. M., Isa, K. M., & Gopinath, S. C. B. (2022). Study on
characterization of bio-oil derived from sugarcane bagasse (Saccharum barberi) for
application as biofuel. Clean Energy, 6(2), 297–304.
https://doi.org/10.1093/ce/zkac012
Ahmad, T., & Zhang, D. (2020). A critical review of comparative global historical energy
consumption and future demand: The story told so far. Energy Reports, 6,
1973–1991. https://doi.org/10.1016/j.egyr.2020.07.020
Almodares, A., & Hadi, M.R. (2009). Production of bioethanol from sweet sorghum: a review.
African J. Agri. 4:772-780.
Austin, K., & Clark, B. (2012). Tearing Down Mountains: Using Spatial and Metabolic
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