Waste Management Bulletin 2 (2024) 288–301

Contents lists available at ScienceDirect

Waste Management Bulletin

journal homepage: www.elsevier.com/locate/wmb

Characterization of phytosynthesized niobium oxide nanoparticle for

efficient conversion of Grewia asiatica L. waste seed oil into sustainable fuel
Rozina a, b, *, Okezie Emmanuel b, c, **, Mushtaq Ahmad a, d, Shaista Jabeen a, Shabeer Ahmad a,
Ahamefula A. Ahuchaogu e
a
Department of Plant Sciences, Quaid- i- Azam University, Islamabad 45320, Pakistan
b
Department of Animal Sciences, College of Food, Agricultural and Environmental Sciences, The Ohio State University, Wooster, OH 44691, USA
c
Department of Biochemistry, Abia State University, PMB 2000, Uturu, Abia State, Nigeria
d
State Key Laboratory, Chinese Academy of Sciences, College of Life Science, Neijiang Normal University, Neijiang 641000, Sichuan, China
e
Department of Pure and Industrial Chemistry, Abia State University, PMB 2000, Uturu, Abia State, Nigeria

A R T I C L E I N F O A B S T R A C T

Keywords: The production of bioenergy and bioproducts from streams of biowaste has ignited interest in fostering a circular
Biodiesel economy worldwide. This study investigates the potential of transforming Grewia asiatica L. waste seed oil into
Grewia asiatica sustainable biodiesel using green-synthesized niobium oxide nanoparticle. Niobium oxide nanocatalyst was
Niobium oxide
synthesized using aqueous leaf extract of Fumaria indica L. Advanced characterization techniques were employed
Seed oil
Sustainable production
to confirm the pure and nano-scale nature of the synthesized niobium oxide nanocatalyst. The synthesized
Transesterification nanocatalyst exhibited an average particle size of 31 nm, resulting in efficient catalytic activity that persited
through the fifth cycle of transesterification. An optimum biodiesel yield of 90% was achieved under reaction
conditions of a methanol to oil molar ratio of 9:1, a reaction time of 180 min, a temperature of 60 ◦ C and a
catalyst load of 0.32 (wt. %). Results of Gas chromatography mass spectrometry (GC–MS) analysis of G. asiatica-
derived biodiesel revealed 5, 8-Octadecadienoic acid methyl ester as the primary fatty acid methyl ester, with the
highest concentration. The fuel properties of G. asiatica-derived biodiesel complied with international standards.
The minimal sulphur content of 0.0001% highlights the clean, environmentally benign and cost-effective nature
of biodiesel synthesized from G. asiatica waste seed oil. This study contributes to the renewable alternative effort
toward transitioning from a linear economy to a circular bioeconomy.

Introduction techniques (Priyadarshini and Abhilash, 2020).

To ensure cost-effective and resource-efficient economic manage­
The use of biomass as a foundational resource for bioenergy pro­ ment, the European Commission introduced the concepts of circular
duction plays a significant role in facilitating the transition from a linear economy and bioeconomy as system models. These models aim to pro­
economy to a circular one, which prioritizes environmental sustain­ duce sustainable energy and mitigate environmental impact by utilizing
ability throughout the production process (Kurniawan et al., 2021). waste biomass. By integrating biofuel technology with the circular
Central to this concept is the belief that the use of renewable materials economy, efforts can be made to protect the environment from biomass
can align industrialization practices with principles of sustainable disposal (Maina et al., 2017). Recycling and reusing materials are
growth and climate stability. In essence, a circular economy seeks to essential tenets of the circular economy, which support a unified bio­
mimic the cyclical processes found in nature by employing ecologically economy by fostering the integration of sustainable biomass resource in
friendly techniques to eliminate waste and minimize energy consump­ industrial applications. The concept of circular economy is built on
tion. Nowadays, there is a growing trend towards designing biode­ bioeconomy, which focuses on the transformation of recyclable carbon
gradable products with low carbon footprints using bio-based pools from biological resources into a range of products like bioenergy

* Corresponding author at: Department of Plant Sciences, Quaid- i- Azam University, Islamabad 45320, Pakistan.
** Corresponding author at: Department of Animal Sciences, College of Food, Agricultural and Environmental Sciences, The Ohio State University, Wooster, OH
44691, USA.
E-mail addresses: [email protected] (Rozina), [email protected] (O. Emmanuel).

https://doi.org/10.1016/j.wmb.2024.05.008

Available online 27 May 2024

2949-7507/© 2024 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

and polymers (Immonen et al., 2020). The circular economy places a transesterification of oil to biodiesel overcomes all these challenges, thus
strong emphasis on minimizing reliance on non-renewable energy attracting attention from researchers for industrial applications (Basu­
sources, such as fossil fuels, and focuses on the sustainable use of natural matary et al., 2021b). Heterogeneous catalysts offer man advantages
resources (Emmanuel et al., 2024). such as low reaction time under optimum conditions with amplified
A circular economy strategy encompasses designs, procedures, and catalytic activity, produce high-quality products, prevent the formation
solutions aimed at maximizing the utilization of side streams within the of soaps during the reaction, have the potential to be employed in
energy sector (Duque-Acevedo et al., 2020; Sheldon, 2020). Increased continuous processes, and are environmentally benign (Basumatary
resource efficiency is one of the main principles of the circular economy. et al., 2018).
It has been demonstrated that the use of renewable resources may lower Recently, nanocatalysts have garnered significant attention in
the cost of utilizing raw materials for industrial purposes (Rekleitis et al., various fields, including wastewater management, optoelectronics and
2020). Additionally, material flows are integral to the definition of cir­ medication delivery. Moreover, nanocatalysts also play a key role in
cular economy (Qin et al., 2021). Hence, the demand for renewable biodiesel synthesis because of their effective catalytic activity, reus­
energy and related services is growing over time to meet basic human ability and high stability (Cao et al., 2021; Ugbogu et al., 2019). Green
needs and drive socioeconomic development (Kurniawan et al., 2021). mediated synthesis of nanoparticles using non-toxic plant extracts as
Biodiesel, composed of a long chain fatty acids, is known for its non- reducing reagents (Ekweogu et al., 2019; Emmanuel et al., 2021;
toxic, biodegradable and eco-friendly properties, being devoid of Ikpeazu et al., 2019; Mbanaso et al., 2020; Ugbogu et al., 2024) is
sulphur and aromatic compounds (Vignesh et al., 2020; Alsaiari et al., preferred over chemical and physical procedure. The synthesis of green
2022). Sources used for biodiesel synthesis includes algae, fungi, edible nanoparticles is innocuous and environmentally safe practice. In
and non-edible seed oils, animal fats, waste cooking oil from domestic chemical synthesis of nanoparticles, stabilizing agents are utilized to
and industrial practices (Bidir et al., 2021; Emmanuel et al., 2022a). prevent aggregation, while in green synthesis, biomolecules such as
Based on kind of sources, biofuels are categorized into four generations. enzymes and amino acids from plant extracts, can function as stabilizing
First-generation biofuels are synthesized using edible seeds, second- and reducing agents (Ugbogu et al., 2020; Yatish et al., 2020; Emmanuel
generation biofuels are derived from non-edible seeds oil, third- et al., 2018; Akubugwo et al., 2022; Emmanuel et al., 2022b; Ugbogu
generation biofuel are extracted from algal sources, while fourth- et al., 2021). These nanocatalysts can be used in various carbon-based
generation biofuels are synthesized from genetically modified algae. conversion reactions.
Due to their environmentally benign impact and renewable nature, non- In comparison to their chemical or physical counterparts, green
edible seeds are highly preferred. Non-edible seeds boast impressive methods for the production of niobium nanoparticles (Nb2O5 NPs) are
production cabilities and have the potential to mitigate the food versus affordable and energy-efficient. Nb2O5 NPs have attracted interest in
fuel competition (Sarkar et al., 2021). both research and industry due to their excellent biocompatibility,
While biofuels serve to lessen reliance on fossil fuels, the synthesis of antibacterial, antioxidant, and anticancer activities, as well as their ca­
biodiesel from edible oils puts the needs for food and fuel at odds with pacity to lower triglyceride and cholesterol levels (Dien et al., 2020;
one another. These glitches can be remedied if non– palatable seed oil is Goswami et al., 2023). The biosynthesis of Nb2O5 NPs in our current
utilized as the feedstock for second-generation biodiesel synthesis investigation was carried out using Fumaria indica L. leaf extract.
instead of edible oil. Several plant species produce non-edible seed oils In the present research, aqueous leaf extract of F. indica was inves­
for methyl ester production as documented in previous studies (Rozina tigated for its efficacy as a stabilizing and reducing agent in the synthesis
et al., 2017a). of phyto-nanocatalysts. The stability and efficiency of the synthesized
Non-edible oils constitute a viable and desirable option for the Nb2O5 NPs to transform novel and non-edible seed oil of G. asiatica into
generation of biodiesel. The proximity of non-edible seed oils is regu­ methyl ester was studied through a series of experiments using Response
lated by the topography, climate, local vegetation, and soil (Rozina surface methodology (RSM). Several analytical techniques like X- ray
et al., 2017a; Rozina et al., 2017b). Currently, over 95 % of commercial diffraction (XRD), fourier-transform infrared spectroscopy (FTIR),
biodiesel produced globally is derived drom vegetable oils. Several non- scanning electron microscopy (SEM) and energy diffraction X-Ray (EDX)
edible seed oils such as Thevetia peruviana Schum (Deka and Basumatary, were used to characterize the newly synthesized Nb2O5 NPs. The syn­
2011), Jatropha curcas (Basumatary et al., 2021a, 2021b), Datura stra­ thesized biodiesel was characterized using innovative techniques like
monium (Koria and Thangaraj, 2010), Cestrum nocturnum (Rozina et al., nuclear-magnetism resonance (NMR), GC–MS, and FTIR. The fuel
2024b), and rubber plants (Roschat et al., 2017) etc., have already been properties of G. asiatica-derived biodiesel were tested and compared
investigated for biodiesel production. with international standards. Hence, G. asiatica-derived biodiesel
In this study, the potential of using Grewia asiatica L., a member of emerges as a novel, environmentally friendly, and economically
the Malvaceae family for biodiesel production was explored. G. asiatica important fuel source with commercial potential.
is distributed in Australia, Bangladesh, China, Sri Lanka, Philippines,
India and Pakistan (Dev et al., 2019). This species is a large shrub or a Research Methodology
small tree with greyish-white bark. Leaves contains hairs on both abaxial
and adaxial surface and are mostly ovate to orbicular in shape. Seeds are Chemicals used and seed oil content determination
ovate in shape and beige in colour. Notably, the non-edible seeds of
G. asiatica are rich source of oil contents hence, it is novel biomass Chemicals used included n-hexane (99.6%) with CAS number
source of biodiesel production at large scale. Our literature evaluation 110–54-3, Niobium(V) chloride (NbCl5) with CAS number 10026–12-7,
indicates that this oil-rich plant species is accessible, inexpensive, and methanol (99.9%) with CAS number 67–56-1 and n-propyl alcohol CAS
novel source for the synthesis of biodiesel. Biodiesel synthesis from non- number 71–23-8. Seeds of G. asiatica were collected during diverse field
edible seeds of G. asiatica has not been reported previously. visits in the summer season from Islamabad Capital Territory, Pakistan.
Among various techniques, catalytic transesterification of tri­ The collected seeds were shade-dried at room temperature (25 ℃) for
glycerides is thought to be the most straightforward and economical way about one week to remove water content (Abbasi et al., 2023). Subse­
to produce biodiesel. several catalysts, including homogeneous, and quently, the seeds were placed inside the oven at 60 ℃ for one day until
heterogeneous catalysts, are used in transesterification (Basumatary they were completely dried.
et al., 2021a, 2022; Rozina et al., 2024b). However, there are some The Soxhlet method was used to determine the oil content (Alsaiari
drawbacks associated to homogeneous and enzyme-catalyzed trans­ et al., 2022). To achieve the actual seed oil content, the seeds were kept
esterification (Kalita et al., 2022). With its quick rate of reaction and in the oven at 60 ◦ C for a whole day to ensure maximum water content
simple separability, the heterogeneous solid base-catalyzed removal. A mortar and pestle were used to crush the seeds into a fine

289
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Table 1
Results of experimental trials of transesterification of Grewia asiatica-derived
biodiesel.
Run A: Alcohol to oil B: Catalyst C: Temperature D: Time Yield
molar ratio loading ◦
C (min)

wt.% wt.
%
1 3:1 0.32 60 60 68
2 3:1 0.32 120 60 65
3 9:1 0.32 120 180 69
4 9:1 0.32 60 120 87
5 15:1 0.32 120 60 64
6 3:1 0.32 60 180 67
7 9:1 0.585 120 120 83
8 15:1 0.32 120 180 64
9 9:1 0.32 120 180 67
10 15:1 0.585 60 120 68
11 9:1 0.32 60 60 60
12 9:1 0.32 60 180 90
13 9:1 0.32 120 180 58
14 9:1 0.585 90 180 77 Fig. 1. XRD pattern of photosynthesized Nb2O5 NPs.
15 15:1 0.32 90 180 70
16 9:1 0.85 90 120 79
17 15:1 0.32 90 60 65
18 9:1 0.32 90 120 65
19 15:1 0.85 60 180 62
20 9:1 0.88 120 180 56 Catalyst synthesis
21 9:1 0.585 60 120 76
22 3:1 0.32 60 120 70 Green Nb2O5 NPs were prepared with aqueous leaf extract of
23 9:1 0.32 60 60 60
F. indica. For this purpose, dust particles were removed from plant leaves
24 3:1 0.85 60 180 65
25 3:1 0.85 60 60 60 of F. indica through thorough cleaning and washing with distilled water.
26 15:1 0.85 120 60 58 About 40 g of plant leaves were taken in a 1000 mL beaker with 500 mL
27 9:1 0.88 60 120 58 of distilled water, and heated at 300 ◦ C on a hotplate for 5 h until the
28 9:1 0.85 60 60 68 volume was reduced by half (Rozina et al., 2021). The prepared plant
29 15:1 0.85 120 180 62
30 15:1 0.85 60 180 70
extract was filtered into the flask by using filter paper fitted in a funnel.
The filtered plant extract was refrigerated at 4 ◦ C for 12 h. To prepare a
200 mM solution of NbCl5, 3 g of NbCl5 was taken and dissolved in 200
powder. About 5 g of powdered G. asiatica seeds were placed in the mL of 60% ethanol for 30 min. About 250 mL of the stored leaf extract
thimble of the Soxhlet apparatus, which has a 250 mL round-bottom was gradually added with the molar solution using a pipette, with
flask, and a reflex condenser. About 90 mL of n-hexane was put in the continuous stirring. The mixture was then heated for 4 h at 50 ◦ C. A dark
round bottle flask and utilised as the solvent. The apparatus was oper­ brown liquid was poured in the petri plates and transferred to an oven
ated at 60 ◦ C for 6 h. During the process, extra solvent was evaporated by for drying at 60 ◦ C to achieve maximum dryness. Using a scraper, the dry
a rotary evaporator to ensure its reusability. The thimble containing the catalyst was removed and placed into crucibles, and calcined at a tem­
powdered seeds was then removed from the Soxhlet device and placed in perature of 450 ℃ for 3.5 h in a muffle furnace (Sathish et al., 2023).
an oven set at 70 ◦ C for a full day to properly dry out and remove any
leftover solvent (Rozina et al., 2022a). The oil content was calculated
Transesterification
gravimetrically using the following formula (Eq. (1)).
Weightofoilproduced To carry out the transesterification process under particular reaction
Weight% = x100 (1)
Weightofsampleused conditions of time and temperature, as well as methanol ratio, amount of
catalyst loading along with measured volume of G. asiatica seed oil was
subjected to Nb2O5 green NPs (Gupta and Agarwal, 2016). Trans­
Free fatty acids content determination esterification of G. asiatica seed oil was carried out in a flask equipped
with a water-cooling system, a reflux condenser, and a magnetic stirrer.
It is required to determine the free fatty acids (FFAs) content before The prepared nano catalyst (0.32 wt%) was mixed in a 6:1 M ratio with
starting transesterification. For this purpose, the acid-base titration methanol and raw G. asiatica seed oil. The transesterification process
method was employed for the calculation of FFAs content in the seed oil. took place at 65˚C for of 3 h. The mixture was centrifuged for 5 min at
A burette was filled with a solution containing 100 mL distilled water 4000 rpm to separate the products from the catalyst. To determine the
and 0.14 g of potassium hydroxide (Chia et al., 2022). Phenolphthalein optimal conditions for transesterification, four independent variables
(two to three drops) was used as an indicator in a round neck flask influencing the biodiesel production during transesterification were
containing G. asiatica seed oil and n-propyl alcohol (1:9). The titration assessed: time (60 to 180 min), temperature (60 to 120 ◦ C), oil to
process was continued until the colour of the oil solution changed into methanolic ratio (3:1 to 15:1), and catalyst loading amount (0.32 to
pink (Rozina et al., 2019). The following Eq. (2) was employed to 0.88 wt%) Table 1. Using the yield percentage equation, the yield per­
calculate FFAs content: centages of glycerol and biodiesel were calculated (Alsaiari et al., 2022).

(Volume used in sample titration − Volume used in blank titration) x KOHconcentration(Lg )

FFA Content = (2)
total volume of oilu sed

290
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Fig. 2. SEM of Nb2O5 NPs.

The yield % of methyl esters was determined using equation (3). heating rate of 10 ◦ C/min.
Analytical techniques, including NMR, GC–MS, and FT-IR spectros­
biodiesel gain (g)
% Yield = x100 (3) copy were used to ascertain physical and chemical characteristics of the
Crude oil utilize (g)
synthesized fatty acid methyl ester. GC–MS analysis was used to
examine the methyl esters and fatty acid content in the synthesized
G. asiatica-derived biodiesel (Teo et al., 2019). The flow rate was set at
Characterization of phyto-nanocatalyst and methyl ester 1.5 mL per minute with a column temperature range of 220–370 ◦ C
utilising helium as a carrier gas. NMR (1H and 13C). of biodiesel sample
Structural characteristics phyto-synthesized Nb2O5 NPs, including was conducted using spectrometer (Bruker) operating at 300 MHz. FT-IR
crystal lattice structure, crystal lattice configuration, and size of particle within a range of 4000–400 cm− 1, and resolution of 1 cm− 1 and 15 cm−
were evaluated through XRD analysis (JOEL JSM 5910 XRD Model). The 1
scans were used to remark the functional group arrangements of
XRD reading of the samples were taken in the range of 2θ = 5–70◦ at a G. asiatica crude seed oil and biodiesel.
rate of 2θ min− 1. The SEM was used to analyse the surface morpholog­
ical characteristics of the potassium oxide nano-catalyst, and EDS was
used to ascertain the chemical makeup of the NPs (Pandya et al., 2022). Statistical analysis
The structural content of Nb2O5 NPs was determined using the FT-IR
analysis within the range of 4000–400 cm− 1. To test the thermal sta­ Software Design Expert 13 was used for central composite design
bility of the nano-catalyst, thermogravimetric analysis (TGA) was con­ (CCD) development which is a division of RSM to examine the influ­
ducted under flowing air conditions, ranging from 55 ◦ C to 1050 ◦ C at a ential role of independent fluctuating conditions during

291
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Fig. 3. EDX spectrum of Nb2O5 NPs.

Fig. 4. FT-IR spectrum of Nb2O5 NPs.

transesterification on plant derived diesel outcomes (Tahir et al., 2019).

Fluctuating conditions such as methanol to oil ratio, time, temperature,
and catalyst amount were defined as independent variables and bio­
diesel yield percentage as variable response. A total of 30 experimental
trials (Table 1) were carried out to investigate the behaviour of the used
variables.

Results and discussion

Catalyst characterization

X-Ray diffraction is a regularly employed method for examining

basic composition, size and crystal phase of nano-catalyst. Fig. 1 shows
Fig. 5. (a) TGA (b) derivative thermogram of Nb2O5 NPs.
the XRD pattern of green Nb2O5 NPs. Energy diffraction peaks at 2θ
values of 9.1◦ , 7.34◦ , 25.60◦ , 26.03◦ , 27.21◦ , 29.05◦ , 36.36◦ , 37.31◦ ,
44.01◦ , 47.62◦ , 48.93◦ , 51.36◦ , 45.21◦ , 46.02◦ , 49.15◦ , 51.14◦ , 55.07◦ , of 25.60◦ (highest peak 110).
58.52◦ , and 59.46◦ corresponded to 301, 304, 110, 405, 402, 313, 803, The reflection peaks revealed a monoclinic phase lettuce structure.
007, 703, 709, 704, 708, 813, and 626 hkl respectively. Crystalline size The average size of NPs in the current study was around 31 nm, which
of Nb2O5 NPs was determined with most deep peak appeared at 2θ value clearly demonstrated that Nb2O5 NPs are nanoscale in nature (Liu et al.,

292
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Table 2 The absorbance of Nb2O5 NPs was measured over the wavelength range
ANOVA results for quadratic model. of 515 cm− 1 to 4000 cm− 1. Fig. 4 shows the FT-IR spectrum of Nb2O5
Source Sum of df Mean F Value p-value NPs. Physiosorbed water molecules (OH stretch) is attributed to the
Squares Square distinctive characteristic absorption at 935 cm− 1, and the strong bands
Model 2294.34 14 163.88 8.41 < 0.0001 at 1478 cm− 1 and 2465 cm− 1 are ascribed to Nb-O stretching. These
significant groups collectively mediate the reduction of Nb2O5 NPs (Dien et al.,
A-Methanol to 32.00 1 32.00 1.64 0.0195 2022).
oil ratio The thermal stability of Nb2O5 NPs was examined using the TGA.
B-Catalyst 45.48 1 45.48 2.33 0.0474
concentration
Fig. 5a shows the thermogram of the synthesized nanoparticles and the
C-Temperature 5.16 1 5.16 0.2645 0.0145 related derivative thermogram (Fig. 5b). Three stages of heat deterio­
D-Time 182.22 1 182.22 9.35 0.0080 ration were visible in both thermograms. At temperatures between 50 ◦ C
AB 3.06 1 3.06 0.1571 0.0074 and 100 ◦ C, 0.86 % of the mass of Nb2O5 NPs was lost during the early
AC 39.06 1 39.06 2.00 0.0173
stage. This loss is related to water removal from the molecular surfaces
AD 3.06 1 3.06 0.1571 0.0274
BC 5.06 1 5.06 0.2597 0.0177 and through evaporation. Thermal degradation (0.98 %) was observed
BD 1.34 1 1.34 0.0688 0.0166 in the second step at temperatures between 110 ◦C and 200 ◦C,
CD 0.0625 1 0.0625 0.0032 0.0456 revealing considerably high thermal stability of Nb2O5 NPs and
A2 662.21 1 662.21 33.98 < 0.0001 enhanced catalytic activity. The NPs underwent additional change (1.36
B2 14.80 1 14.80 0.7595 0.0372
C2 93.83 1 93.83 4.81 0.0444
%) in the third stage, which happened at temperatures between 201 ◦ C
D2 11.67 1 11.67 0.5989 0.0410 and 950 ◦ C. In Fig. 5b endothermic peaks of derivative curve (wt.%), are
Residual 292.36 15 19.49 clearly visible.
Lack of Fit 145.36 10 14.54 0.4944 0.8394 not
significant
Pure Error 147.00 5 29.40 Biodiesel synthesis via transesterification
Cor Total 2586.70 29
2
R = 0.8870, Std. Dev. = 4.41, C.V. % = 8.09, Adeq Precision = 10.299 In this study, Nb2O5 NPs was used to synthesize methyl ester from a
novel non-edible G. asiatica seed oil. Compared to other reported spe­
cies, the seed oil content of was 25 % of the total dry weight (Ong et al.,
2021). A single step transesterification reaction was produced by seed
oil, which had a significantly reduced FFA content of 0.72 (wt.%). An
FFA content exceeding 3% in seed oil is considered undesirable and
requires an additional step of acid transesterification, which limits the
concentration of triglycerides that may be converted to methyl esters
during the transesterification reaction (Allami, et al., 2023). As a result,
G. asiatica L. seed oil can be efficiently used to produce methyl ester in a
single step.
RSM was extensively used to determine the optimum reaction con­
ditions for achieving the highest possible yield of methyl ester. As shown
in Tables 2, the CCD was created using four independent trans­
esterification variables. Fig. 6 shows that the predicted and actual values
of methyl ester yield are distributed quite close to the straight line.
Comprehensive findings from the statistical analysis of variance of the
model are shown in Table 2. The significance of the quadric model was
determined with a low p-value of 0.0001. In addition, the most signifi­
cant term among the quadratic terms of the transesterification catalyst
loading (A2) had a p-value of 0.0001 and was followed by catalyst load
(B2). With sufficient precision, we were able to determine the model’s
signal-to-noise ratio, which was found to be 10.299 in the present study,
indicating that the experimental model can accurately predict methyl
ester yield. A desirable ratio is one that is greater than 4 (Sharma et al.,
Fig. 6. Relationship between the experimental and predicted biodiesel yield. 2023). The polynomial Eq. (4) used in the experimental model is given
below.
2022). Results of X-Ray diffraction of Nb2O5 NPs were found in agree­
ment with the SEM. The SEM was used to examine the surface BiodieselYield(wt.%) = + 81.22 − 1.33*A − 1.61*B + 0.5251*C
morphology of green nanoparticles of Nb2O5 NPs. The topology of nano- + 2.98*D + 0.4375*AB − 1.56*AC
catalyst was observed to have a uniform cubical shape. Fig. 2 shows a + 0.4375*AD − 0.5625*BC − 0.2846*BD (4)
SEM micrograph revealing a predominantly rectangular and largely − 0.0625*CD − 14.92*A2 + 2.54*B2
homogeneous particle structure. However, due to the agglomeration of
− 5.19*C2 + 1.82*D2
smaller NPs during the SEM examination, larger NPs are also observed
(Sharma et al., 2023).
The chemical makeup of the synthesized NPs was identified using Cumulative effect of reaction variables on transesterification
EDX. Peaks corresponding to Nb and O observed in the spectrum pro­
vided evidence of the formation of Nb2O5 NPs (Fig. 3). Nb and O Transesterification is significantly influenced by the mutual inter­
comprised 25.22 % and 74.88 % of the total composition, respectively. action between catalyst amount and Met:Oil (Fig. 7a). The highest
The lack of additional unnecessary peaks in the EDX spectrum confirmed production of 90 % biodiesel was seen at a catalyst amount of 0.32 (wt.
the purity and lack of other elements in green NPs. %), a Met:Oil of 9:1, 180 min, and a temperature of 60 ◦C (Run 12). At
The FTIR spectrum of Nb2O5 NPs was obtained in absorbance mode. Run 19, the synthesis of methyl ester decreased by 62 % because of
higher catalyst concentration of 0.85 (wt. %) and higher Met:Oil of 15:1.

293
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Fig. 7. Impact of the reaction conditions of G. asiatica-derived biodiesel.

At Run 10, a catalyst loading of 0.58 (wt. %) with a Met:Oil of 15:1 maximum output of 70 % was attained at 90 ◦C with a Met:Oil of 15:1 at
resulted in a low yield of 68 %. When the amount of methanol in the Run 15. The excess of methanol is blamed for the rise in methyl ester
reactant mixture exceeds the optimal level, it thins the concentration of yield because it stimulates the catalyst to produce methoxy species,
the catalyst, favouring reversible reactions (Naveenkumar and Baskar, which drive the reaction in forward direction (Bohlouli and Mahdavian
2020). Low yield of 67 % was added by a lower Met:Oil of 3:1 and a 2019). Results of the experimental investigation showed that a constant
catalyst amount of 0.32 (wt.%) (Run 6). The findings of the ANOVA rise in temperature has a significant impact on reaction rate. The FAME
verified the significant relationship these variables with a p-value of yield drops to 64 % at Run 8 due to higher molar ratios of 15:1 and 120
0.0074. ◦C. This correlation was substantial according to the ANOVA results (p-
Fig. 7b shows the impact of the ratio of Met:Oil and temperature on value 0.0173).
the methyl ester yield those results. A higher yield of 90 % was obtained The Met:Oil and time have a substantial interaction effect on the
at optimum temperature of 60 ◦C, the ratio of Met:Oil was 9:1. (Run 12). generation of biodiesel (Fig. 7c). The catalyst loading of 0.32 (wt.%)
At Run 3, the same Met:Oil (6:1) and 120 ◦ C produced an 69 % yield. A with a Met:Oil of 9:1 produced the highest output of biodiesel, 90 %

294
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Fig. 8. FT-IR spectra of (a) G. asiatica seed oil and (b) G. asiatica-derived biodiesel.

(Run 12). At reaction time 120 (min), yield was slightly reduced to 87 % yield of 56 % was obtained (Run 20). However, the extra catalyst con­
with the same Met:Oil (Run 4). Yield decreased even further, to 65 %, at centration over this threshold reduced the FAME yield due to an increase
Met:Oil 15:1 and 60 (min) (Run 17).A surplus of alcohol increases the in reaction mixture viscosity and a decrease in catalytic activity, which
solubility of glycerol, making biodiesel purification challenging (Mokbli reduced interaction between the catalyst and reactants and caused a low
et al., 2021). At Met:Oil 6:1 and time 55 (min), around 64 % yield was product concentration (Ambat et al., 2020). Combination impact was
attained (Run 19). It unquestionably led to partial conversion and a low deemed significant by having a p-value of 0.0177. The combined impact
FAME yield because there was not time to adequately combine the re­ of time and catalyst load on FAME synthesis is depicted in a 3D form in
actants and reach equilibrium going forward (Feyzi and Shahbazi 2019). Fig. 7e. The maximum biodiesel production of 90 % was attained after
A low Met:Oil ratio of 3:1 and time 120 (min), the minimum yield of 70 180 min at a constant Met:Oil of 9:1 at a temperature of 60 ◦C. (Run 12).
% was attained (Run 18). A yield of nearly 76 % was attained with a nano catalyst concentration of
Fig. 7d illustrates the impact of mutual interaction between catalyst 0.58 (wt.%)) and a run time of 120 min (Run 21).
loading, temperature, at constant Met:Oil of 9:1and the and time (180 It can be proven that the reaction time was too short to achieve
min) on transesterification. With a temperature of 120 ◦C and a reduced chemical equilibrium and that the catalyst needed time to interact,
catalyst loading of 0.32 wt%, about 67 % yield was produced (Run 9). It resulting in a lower-quality product. After 2 h, the forward reaction was
is believed that the minimum boiling point of alcohol is to blame for the in full swing, equilibrium had been reached, and a maximum conversion
transesterification’s forward reaction being slowed down. At Run 14, a yield of 90 % had been noted at run 12. With a longer reaction period, a
temperature of 90 ◦C and a Nb2O5 load of 0.58 wt% resulted in about 77 steady elevation in FAME yield was observed. At a fix Met:Oil (9:1) and
% yield (Run 14). When MgO concentration was increased from 0.5 to 2 catalyst loading (0.32 wt%), the highest productivity of 90 % biodiesel
%, it was shown to improve the yield of FAME in soybean oil (Elkelawy was attained in 180 min at 60 ◦C (Run 12). From Run 18 with time 120
et al., 2019). However, as concentration increased further, the yield of min and temperature 90 ◦ C, about 65 % of the yield was revealed. Time
biodiesel declined. Thus, their findings are in complete agreement with of 180 min at a high temperature of 120 ◦C resulted in a further 58 %
the findings of our current investigation (Elkelawy et al., 2019). At the reduction in methyl ester synthesis (Run 13). This investigation revealed
highest Nb2O5 load of 0.88 wt% and temperature of 120 ◦C, a minimum that reaction productivity increased with rising temperature and

295
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Fig. 9. NMR spectrum of (a) 1HNMR and (b) 13

CNMR of Grewia asiatica biodiesel.

reaction duration up to a certain point. These two variables are signif­ 1160.26 cm− 1.
icant per ANOVA results with a p-value (<0.05). A very variable portion of the oil and biodiesel spectra was found
between 1000 and 2000 cm− 1 and 3300 and 2800 cm− 1. The resulting
Characterization of G. asiatica-derived biodiesel stretch peak in the spectra at 1098.06 cm− 1 was the wagging frequency
for C-H2 (Ameen et al., 2022). When compared to the spectrum of
FT-IR methyl ester, deep peaks at 3321.97 cm− 1 that spotted in the spectrum of
One of the widely utilized methods for examining the structural G. asiatica seed oil vanished in FAME spectrum. In the spectra of methyl
composition of biodiesel is FTIR spectroscopic analysis. Once trans­ ester, the deep stretch for (O–H) at 1023.10 cm− 1 was gone. These
esterification is complete, FTIR aids in the confirmation of methyl ester analysed peaks on the spectrum of methyl ester and seed oil from
production along with NMR analysis. Fig. 8 a and b, which show the G. asiatica have confirmed that transesterification converts oil tri­
FTIR spectra of synthetic methyl ester and oil from G. asiatica, respec­ glycerides into methyl esters.
tively. In the biodiesel spectrum, a key band for the carbonyl group (C =
1
O) could be seen at 1743.52 cm− 1 in the infrared, while a band for the HNMR
methyl group (CH3) could be seen at 1464.47 cm− 1. These two bands’ The 1HNMR spectroscopic approach was used to confirm production
presence is proof that methyl ester formed at the conclusion of trans­ of G. asiatica-derived biodiesel. Fig. 9a depicts the corresponding
esterification (Rozina et al., 2024a; Rozina et al., 2017b). Stretch for CH absorbance peak of the G. asiatica-derived biodiesel 1HNMR spectrum.
(sp2) was observed at 2853.31 cm− 1, while the characteristic peak of The 1HNMR spectrum of biodiesel revealed a distinctive peak for the
C–H (sp3) occurred in the IR region at 2922.62 cm− 1. The carbonyl methoxy group (− OCH3) at 3.671 ppm, indicating effective trans­
group’s IR region is thought to be the most susceptible to chemical and esterification and subsequent methyl ester synthesis. In the 1HNMR
molecular changes in the biodiesel spectrum of all the other peaks spectra of G. asiatica-derived biodiesel, no unwanted methanol signal
(Rozina et al., 2021). Stretch (O = C-O-C) for aliphatic esters detected at was found. Typically, it is detected around 3.45 ppm.

296
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Fig. 10. GC–MS spectrum of G. asiatica-derived biodiesel.

The proton peak for the triplet methylene (–CH2) in the 1HNMR hydrogen was responsible for the peak that was seen at 2.557–2.777
spectra of G. asiatica-derived biodiesel was discovered at 2.283–2.333 ppm (–CH2). These 1HNMR peaks have demonstrated the existence of
ppm. At 1.261–1.309 ppm, a singlet-like peak for –CH2 protons was seen methyl esters in the biodiesel sample. The entire conversion of tri­
in the spectra. The hydrogen element on the C-3 of corresponds to these glycerides into FAME was calculated and it was found to be 90 %.
protons of − methylene. peak of incorporated terminal methyl protons at The position of the esters –COO- and C-O group, as well as other
0.810–0.918 ppm. The signal observed at 5.310–5.401 ppm was olefinic structural details, were explored using the biodiesel from G. asiatica
13
hydrogen, which has two carbon atoms linked by a double bond. Allylic CNMR spectrum. Fig. 3.8.9b shows the 13CNMR spectrum of

297
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Table 3 peaks were further confirmed by MS analysis using the library match
Comparison of G. asiatica-derived biodiesel fuel properties with IS. program NO. NIST02. Hexadecanoic acid methyl ester (C16:0), tride­
Property Methods Grewia asiatica ASTM D- EN- China GB/T canoic acid methyl ester (C14:0) and Octadecanoic acid, methyl ester
6751 14214 20828–2007 (C18:0) were both found in saturated methyl esters. Unsaturated methyl
Mean St.
Dev. ester composed of 5, 8-Octadecadienoic acid methyl ester (C18:2), and
9-Octadecenoic acid, (2)-methyl-, methyl ester (C18:1). The chromato­
Color Visual 2.0 2.0
gram with the highest abundance of 5, 8-Octadecadienoic acid methyl
−
Acid ASTM- 0.200 0.1 ≤0.5 ≤0.8 ≤0.5
number D974 ester at retention time 11.81 min was found to be a significant fatty acid
(mg methyl ester. Typically, a biodiesel sample with a high degree of satu­
KOH/g) ration is thought to be advantageous for obtaining the highest oxidative
Flash ASTM- 97 14 ≥93 ≥130 ≥120
stability (Akram et al., 2022; Rozina et al., 2022a, 2022b). Nevertheless,
Point D93
(◦ C) biodiesel high in polyunsaturated methyl esters has less oxidative sta­
Pour Point ASTM- − 6 5 − 15–16 _ _ bility but more attractive cold flow characteristics (Atabani et al., 2013).
(◦ C) D97 The methyl ester of G. asiatica has been shown by GC-MS analysis to be a
Viscosity ASTM- 3.76 0.5 1.9–6.0 _ 3.4–5.0 very capable renewable energy source.
(mm2/s D445
at
40 ◦ C.) Fuel properties of G. asiatica-derived biodiesel
Density ASTM- 0.84 1.06 ≤0.86 _ ≤120
(kg/m3 D1298 Prior to practical application, it is necessary to do an analysis of the
at 40 ◦ C)
fuel qualities of a sample of synthetic methyl ester that must be com­
Sulphur ASTM- 0.0001 1 ≤0.05 ≤0.05 ≤0.20
content D4294 parable to international standards (IS). The structure of the fatty acid
(wt.%) profile in the seed oil used for transesterification has a significant impact
Cloud ASTM- − 9 1 − 3.0–12 _ _ on the physiochemical properties of biodiesel (Amenaghawon et al.,
point D2500
2022). Table 3 lists the biodiesel fuel qualities of G. asiatica-derived
(◦ C)
biodiesel that were investigated.
Acid value has a significant impact on the quality of fuel. The acid
value of biodiesel therefore has a significant impact on engine perfor­
Table 4 mance. In order to neutralize the FFA present in liquid fuel, a certain
Comparison of the catalytic activity of Nb2O5 with previous research. amount of potassium hydroxide is needed, and this is what it denotes.
Feedstock Method of Catalyst Maximum References Old diesel engines’ rubber components experience problems and
Transesterification Used number of corrode when biodiesel’s acid value exceeds the permitted level. The
reusability methyl ester of G. asiatica had an acid value of 0.200 (mg KOH/gm),
cycle which lies within the range of fuel that is generally acceptable on a
Sunflower Conventional CaO–Au 10 Amesho global scale.
seed oil et al., 2022 Kinematic density significantly affects the fuel property of biodiesel,
Cestrum Conventional Sb2O3 5 Rozina
which directly regulates engine performance, fuel flow through pipeline
nocturnum et al.,
seed oil 2024b systems, and injector nozzles. The viscosity of biodiesel is increased by
Saussurea Conventional ZrO2 5 Alsaiari, fuels with higher density, which causes incomplete combustion and
heteromalla etal., 2016 increased particulate matter generation (Tamjidi et al., 2021). Kine­
Jatropha Conventional CaSO4/ 4 Teo et al., matic density G. asiatica-derived biodiesel, which was determined to be
curcas Fe2O3- 2019
SiO2
0.84 (mm2/s), equivalent to international fuel criteria.
Sunflower Conventional MgO/ 5 Alaei et al., Fuel atomization is significantly influenced by the kinematic vis­
seed oil MgFe2O4 2018 cosity of the fuel. Lower viscosity fuel results in leakage issues and
Cupressus Conventional TeO2 5 Rozina provides less lubrication for injection pumps, which leads to increased
sempervirens et al.,
power loss in the fuel engine. Similarly, high viscosity ensures inade­
seed oil 2024c
Grewia Conventional Nb2O5 5 Present quate fuel supply for the injection pump and subsequent engine effi­
asiatica work ciency (Ganesan et al., 2021). Kinematic viscosity of Grewia asiatica in
seed oil the current experiment was 3.76 (mm2/s), which lies the range of the IS.
The term “flash point” refers to the temperature at which fuel begins
to burn when an ignition source is present. Fuel having a greater flash
G. asiatica-derived biodiesel that has been manufactured. Methoxy car­
point has a low risk of catching fire accidentally during storage and
bon was defined in the 13CNMR spectra by a peak at 51.42 ppm. At
transportation (Borah et al., 2019). In comparison to traditional fossil
174.06 ppm, a signal for the carbonylic group (–COOH) was detected
fuels, biodiesels have greater flash points, making them safer to handle
(Bano et al., 2020). The peak at 127.80–128.01 ppm, which represented
(Rozina et al., 2022a). According to Table 3 the biodiesel made from
the internal non-conjugated carbon atoms, allowed for the detection of
Grewia asiatica had a flash point of 97 ◦ C.
the degree of unsaturation, which is represented by –CH = CH–, in the
The pour and cloud points of the gasoline affect how well diesel
biodiesel sample. Additionally, chemical shifts seen between ppm values
engines work in colder parts where temperature drops into the nega­
129.70 to 130.13 ppm showed that the 13CNMR spectra contained
tives. The fatty acid makeup of oil used in transesterification directly
exterior carbons of non-conjugated carbons (–CH = CH–). C-O group
influences the pour point of the biodiesel produced (Rozina et al.,
signal was detected between 76.60 to 77.482 ppm.
2022b). The biodiesel produced from Grewia asiatica had a pour point of
− 6 ◦ C, which complied with international fuel regulations. The biodiesel
GC-MS
temperature at which fuel crystallization begins is referred to as the
The FAME profile significantly affects biodiesel quality. The ester
cloud point. In this study cloud point of was − 9 ◦C, equivalent to the IS
components of the biodiesel sample were identified for this purpose
of fuel. In comparison to petro-diesel, which has a sulphur concentration
using GC-MS analysis. Fig. 10 shows the gas chromatogram of Grewia
of 50 ppm, G. asiatica-derived biodiesel sulphur content was determined
asiatica-derived biodiesel, which exhibits five distinct peaks. These
to be 0.0001 %. This small amount of sulphur improves the quality of the

298
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Fig. 11. Reusability of Nb2O5 NPs in transesterification.

biodiesel, making it environmentally friendly (Talavari et al., 2021). temperature of 60 ◦C. The chromatogram of the synthesized biodiesel
revealed five distinct peaks of FAMES. The methyl ester of 5, 8-Octade­
Catalyst reusability cadienoic acid was observed to be the main methyl ester, with highest
concentration. The fuel related characteristics of G. asiatica-derived
The ability of Nb2O5 NPs to be recycled was investigated to assess its biodiesel were comparable to international fuel standards i.e., density
stability and economic sustainability in subsequent cycles of trans­ (0.84 kg/m3), viscosity 3.76 mm2/s), flash point (97 ◦ C), cloud (− 9 ◦ C),
esterification. The methods used to clean and separate the catalyst from and pour point (− 6 ◦ C). It can be concluded from the current study that
the reaction mixture have a significant impact on the catalyst’s ability to G. asiatica possesses significant potential for environmental remediation
be reused (Rozina et al., 2024a). Reusability of the generated Nb2O5 NPs through the utiliziation of its waste seed in the production of eco-
was carried out under ideal transesterification reaction conditions, friendly biodiesel. Nonetheless, further research is recommended to
including Met:Oil ratio of 9:1, catalyst loading of 0.32 (wt.%), reaction evaluate the economic feasibility and engine efficiency of G. asiatica-
time of 180 min, and temperature of 60 ◦C. derived biodiesel through comprehensive testing.
After the first cycle of transesterification, green NPs of Nb2O5 were
recovered from the reaction mixture by centrifugation. The recovered CRediT authorship contribution statement
particles were then cleaned with alcohol to remove impurities, dried in
the oven, and then calcined for 180 min at 500 ◦ C in the muffle furnace Rozina: . Okezie Emmanuel: Writing – review & editing, Writing –
and stored after preparation for reuse in the following transesterification original draft, Conceptualization, Data curation, Investigation. Mushtaq
cycles. Catalytic activity was investigated up to seven cycles. The Ahmad: Writing – review & editing, Supervision. Shaista Jabeen:
maximum catalytic performance was observed up to five consecutive Software, Resources, Writing – review & editing. Shabeer Ahmad:
cycles producing high FAME yields of 90 to 70 %. The catalytic activity Writing – review & editing, Software. Ahamefula A. Ahuchaogu:
of Nb2O5 NPs is compared with previous studies and presented in Investigation, Methodology, Writing – review & editing.
Table 4. A decline in methyl ester production was observed up to 70 % in
the fifth cycle. Yield fell even more up to 60 % in the sixth cycle and 55 Declaration of competing interest
% in the seventh (Fig. 11).
Chemical analysis indicates that the drop-in catalytic activity is due The authors declare that they have no known competing financial
to the poisoning of Nb2O5 NP sites by organic components present in the interests or personal relationships that could have appeared to influence
transesterification mixture, leading to a decreased methyl ester pro­ the work reported in this paper.
duction. Nevertheless, after washing and calcination in a muffle furnace,
the catalytic activity of the NPs can be recovered. Acknowledgements

Conclusions The authors extend their gratitude to the Higher Education Com­
mission (HEC) of Pakistan for providing Ms. Rozina with a fellowship to
Given the current global environmental challenges, such as global conduct research at The Ohio State University, United States. Addi­
warming, and energy depletion, there is a pressing need to explore and tionally, the authors express appreciation for the financial assistance to
develop more environmentally friendly and renewable energy sources. Mr. Okezie Emmanuel received from the U.S. National Science Foun­
Utilizing waste and non-edible feedstocks to produce biodiesel can help dation Research Traineeship EmPOWERment Program, granted under
alleviate burden on the environment. In the current study, non-edible award number 1922666.
seed oil derived from G. asiatica was utilized for biodiesel synthesis via
transesterification, employing phytosynthesized Nb2O5 NPs in the pro­
cess. The highest biodiesel yield of 90% was achieved at a catalyst
loading of 0.32 (wt. %), a Met:Oil ratio of 9:1, 180 min, and a

299
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

References Emmanuel, O., Uche, M.E., Dike, E.D., Etumnu, L.R., Ugbogu, O.C., Ugbogu, E.A., 2022b.
A review on Garcinia kola Heckel: Traditional uses, phytochemistry, pharmacological
activities, and toxicology. Biomarkers 27 (2), 101–117.
Akram, F., ul Haq, I., Raja, S.I., Mir, A.S., Qureshi, S.S., Aqeel, A., Shah, F.I., 2022.
Ganesan, R., Subramaniam, S., Paramasivam, R., Sabir, J.S., Josephin, J.F.,
Current trends in biodiesel production technologies and future progressions: A
Brindhadevi, K., Pugazhendhi, A., 2021. A study on biofuel produced by catalytic
possible displacement of the petro-diesel. J. Clean. Prod., 133479
cracking of mustard and castor oil using porous Hβ and AlMCM-41 catalysts. Sci.
Akubugwo, E.I., Emmanuel, O., Ekweogu, C.N., Ugbogu, O.C., Onuorah, T.R.,
Total Environ. 757, 143781.
Egeduzu, O.G., Ugbogu, E.A., 2022. GC-MS Analysis of the Phytochemical
Goswami, T., Kumar, S., Bheemaraju, A., Reddy, K.M., Sharma, A.K., Kataria, A.,
Constituents, Safety Assessment, Wound Healing and Anti-Inflammatory Activities of
Shrivastav, A., 2023. TiO2 Nanoparticles and Nb2O5 Nanorods Immobilized rGO for
Cucurbita pepo Leaf Extract in Rats. Sci. Pharm. 90 (4), 64.
Efficient Visible-Light Photocatalysis and Catalytic Reduction. Catal. Lett. 153 (2),
Alaei, S., Haghighi, M., Toghiani, J., Vahid, B.R., 2018. Magnetic and reusable MgO/
605–621.
MgFe2O4 nanocatalyst for biodiesel production from sunflower oil: influence of fuel
Gupta, J., Agarwal, M., 2016. Preparation and characterizaton of CaO nanoparticle for
ratio in combustion synthesis on catalytic properties and performance. Ind. Crop.
biodiesel production. AIP Conference Proceedings Vol. 1724, No. 1.
Prod. 117, 322–332.
Ikpeazu, V.O., Emmanuel, O., Ekweogu, C.N., Akara, E.U., Ugbogu, 2019. A comparative
Allami, H.A., Nayebzadeh, H., Motamedi, S., 2023. The effect of biodiesel production
nutritional assessments of leaf extracts of Ocimum gratissimum and Solanum
method on its combustion behavior in an agricultural tractor engine. Environ. Sci.
aethiopicum. American Journal of Biomedical Research 7 (2), 27–31.
Pollut. Res. 30 (3), 5955–5972.
Immonen, M., Maina, N.H., Wang, Y., Coda, R., Katina, K., 2020. Waste bread recycling
Alsaiari, M., Rozina, A.M., Zafar, M., Sultana, S., Rizk, M.A., Almohana, A.I., Ahmad, Z.,
as a baking ingredient by tailored lactic acid fermentation. Int. J. Food Microbiology
Alsaiari, R.A., Akhtar, M.S., 2022. Treatment of Saussurea heteromalla for biofuel
327, 108652.
synthesis using catalytic membrane reactor. Chemosphere 35335.
Kalita, P., Basumatary, B., Saikia, P., Das, B., Basumatary, S., 2022. Biodiesel as
Ambat, I., Srivastava, V., Iftekhar, S., Haapaniemi, E., Sillanpää, M., 2020. Effect of
renewable biofuel produced via enzyme-based catalyzed transesterification. Energy
different co-solvents on biodiesel production from various low-cost feedstocks using
Nexus 6, 100087.
Sr–Al double oxides. Renew. Energy 146, 2158–2169.
Koria, L., Thangaraj, T., 2010. Optimization of biodiesel production process in Datura
Amenaghawon, A.N., Obahiagbon, K., Isesele, V., Usman, F., 2022. Optimized biodiesel
stramonium seed oil, a non-edible oil source. J. Ecobiotechnol. 2 (5).
production from waste cooking oil using a functionalized bio-based heterogeneous
Kurniawan, S.B., Ahmad, A., Said, N.S.M., Imron, M.F., Abdullah, S.R.S., Othman, A.R.,
catalyst. Cleaner Engineering and Technology 8, 100501.
Purwanti, I.F., Hasan, H.A., 2021. Macrophytes as wastewater treatment agents:
Bano, S., Ganie, A.S., Sultana, S., Sabir, S., Khan, M.Z., 2020. Fabrication and
Nutrient uptake and potential of produced biomass utilization toward circular
optimization of nanocatalyst for biodiesel production: an overview. Front. Energy
economy initiatives. Sci. Total Environ. 790, 148219.
Res. 8, 579014.
Liu, Y., Hong, D., Chen, M., Su, Z., Gao, Y., Zhang, Y., Long, D., 2022. Synergistic action
Basumatary, B., Das, B., Nath, B., Basumatary, S., 2021a. Synthesis and characterization
of Pt and Nb2O5 ultrafine nanoparticles for bidirectional conversion of polysulfides
of heterogeneous catalyst from sugarcane bagasse: production of jatropha seed oil
in high-performance lithium-sulfur cells. Chem. Eng. J. 430, 132714.
methyl esters. Current Research in Green and Sustainable Chemistry 4, 100082.
Maina, S., Kachrimanidou, V., Koutinas, A., 2017. A roadmap towards a circular and
Basumatary, S., Nath, B., Kalita, P., 2018. Application of agro-waste derived materials as
sustainable bioeconomy through waste valorization. Curr. Opin. Green Sustainable
heterogeneous base catalysts for biodiesel synthesis. J. Renewable Sustainable
Chem. 8, 18–23.
Energy 10 (4).
Mbanaso, E., Nwankwo, A., Ijioma, S., Emmanuel, O., Ugbogu, E., Nwagbara, N.,
Basumatary, S., Nath, B., Das, B., Kalita, P., Basumatary, B., 2021b. Utilization of
Ugwuanyi, K., 2020. Haematoprotective and RBC membrane stabilizing effects of
renewable and sustainable basic heterogeneous catalyst from Heteropanax fragrans
Justicia carnae leaf extracts in sodium nitrate intoxicated Wistar rats. Journal of Basic
(Kesseru) for effective synthesis of biodiesel from Jatropha curcas oil. Fuel 286,
and Clinical Physiology and Pharmacology 32 (1), 20190275.
119357.
Mokbli, S., Sbihi, H.M., Nehdi, I.A., Azam, M., Fadhila, A., Romdhani-Younes, M., Al-
Basumatary, S.F., Patir, K., Das, B., Saikia, P., Brahma, S., Basumatary, B., Nath, B.,
Resayes, S.I., 2021. Chemical and fatty acid compositions of crude and purified
Basumatary, B., Basumatary, S., 2022. Production of renewable biodiesel using
extracts obtained from Datura innoxia seeds extracted with different solvents. J. Oleo
metal organic frameworks based materials as efficient heterogeneous catalysts.
Sci. 70 (3), 321–332.
J. Clean. Prod. 358, 131955.
Naveenkumar, R., Baskar, G., 2020. Optimization and techno-economic analysis of
Bidir, M.G., Millerjothi, N.K., Adaramola, M.S., Hagos, F.Y., 2021. The role of
biodiesel production from Calophyllum inophyllum oil using heterogeneous
nanoparticles on biofuel production and as an additive in ternary blend fuelled diesel
nanocatalyst. Bioresour. Technol. 315, 123852.
engine: A review. Energy Rep. 7, 3614–3627.
Ong, H.C., Tiong, Y.W., Goh, B.H.H., Gan, Y.Y., Mofijur, M., Fattah, I.R., Chong, C.T.,
Cao, X., Xu, H., Li, F., Zou, Y., Ran, Y., Ma, X., Cao, Y., Xu, Q., Qiao, D., Cao, Y., 2021.
Alam, M.A., Lee, H.V., Silitonga, A.S., Mahlia, T.M.I., 2021. Recent advances in
One-step direct transesterification of wet yeast for biodiesel production catalyzed by
biodiesel production from agricultural products and microalgae using ionic liquids:
magnetic nanoparticle-immobilized lipase. Renew. Energy 171, 11–21.
Opportunities and challenges. Energ. Conver. Manage. 228, 113647.
Deka, D.C., Basumatary, S., 2011. High quality biodiesel from yellow oleander (Thevetia
Pandya, H.N., Parikh, S.P., Shah, M., 2022. Comprehensive review on application of
peruviana) seed oil. Biomass Bioenergy 35 (5), 1797–1803.
various nanoparticles for the production of biodiesel. Energy Sources Part A 44 (1),
Dev, R., Kannan, V., Kumar, M.S., Dayal, D., Patel, R., 2019. Grewia species: diversity,
1945–1958.
distribution, traditional knowledge and utilization. Wild Fruits: Composition,
Priyadarshini, P., Abhilash, P.C., 2020. Circular economy practices within energy and
Nutritional Value and Products, pp. 395–426.
waste management sectors of India: A meta-analysis. Bioresour. Technol. 304,
Dien, L.X., Truong, Q.D., Murayama, T., Chinh, H.D., Taketoshi, A., Honma, I.,
123018.
Haruta, M., Ishida, T., 2020. Gold nanoparticles supported on Nb2O5 for low-
Qin, L., Wang, M., Zhu, J., Wei, Y., Zhou, X., He, Z., 2021. 2021. Towards circular
temperature CO oxidation and as cathode materials for Li-ion batteries. Appl. Catal.
economy through waste to biomass energy in Madagascar, Complexity.
A 603, 117747.
Roschat, W., Siritanon, T., Yoosuk, B., Sudyoadsuk, T., Promarak, V., 2017. Rubber seed
Duque-Acevedo, M., Belmonte-Ureña, L.J., Plaza-Úbeda, J.A., Camacho-Ferre, F., 2020.
oil as potential non-edible feedstock for biodiesel production using heterogeneous
The management of agricultural waste biomass in the framework of circular
catalyst in Thailand. Renew. Energy 101, 937–944.
economy and bioeconomy: An opportunity for greenhouse agriculture in Southeast
Rozina, Emmanuel, O., Ezeji, T.C., 2024a. Exploring the synergy of nanomaterials and
Spain. Agronomy 10 (4), 489.
microbial cell factories during biohydrogen and biobutanol production from
Ekweogu, C.N., Ude, V.C., Nwankpa, P., Emmanuel, O., Ugbogu, 2019. Ameliorative
different carbon sources. In: Sustainable Chemistry for the Environment, p. 100098.
effect of aqueous leaf extract of Solanum aethiopicum on phenylhydrazine-induced
Rozina, Mushtaq, A., Ezeji, T.C., Emmanuel, O., Qureshi, N., Khan, A., 2024b. Utilization
anaemia and toxicity in rats. Toxicological Research 1–12.
of waste seed oil from Cestrum nocturnum as a novel source for cleaner production of
Elkelawy, M., Bastawissi, H.A.E., Esmaeil, K.K., Radwan, A.M., Panchal, H.,
biodiesel using green nano-catalyst of antimony oxide. Fuel 364, 131124.
Sadasivuni, K.K., Ponnamma, D., Walvekar, R., 2019. Experimental studies on the
Rozina, Emmanuel, O., Ahmad, M., Ezeji, T.C., Qureshi, N., Abidin, S.Z.U., 2024c.
biodiesel production parameters optimization of sunflower and soybean oil mixture
Bioenergy production from waste seed oil biomass of Cupressus sempervirens: A
and DI engine combustion, performance, and emission analysis fueled with diesel/
strategy for reducing environmental pollution. Sustainable Chemistry One World,
biodiesel blends. Fuel 255, 115791.
100008.
Emmanuel, O., Rozina, Ezeji, T.C., 2024. Utilization of biomass-based resources for
Rozina, A.M., Zafar, M., 2021. Conversion of waste seed oil of Citrus aurantium into
biofuel production: A mitigating approach towards zero emission. Sustainable
methyl ester via green and recyclable nanoparticles of zirconium oxide in the context
Chemistry One World, 100007.
of circular bioeconomy approach. Waste Manage. 136, 310–320.
Emmanuel, O., Ugbogu, A.E., Uwadinachi, A., Okeke, S., Achuluno, V., 2018.
Rozina, A.M., Zafar, M., Ali, N., 2019. Biodiesel synthesis and physiochemical analysis of
A comparative study on micronutrients and antinutrients of leaf extracts of
Taraxacum officinale FH Wigg seed oil. Int. J. Environ. Sci. Technol. 16 (8),
Pterocarpus soyauxii and Pterocarpus santalinoides. Journal of Complementary
4103–4112.
Medicine Research 7 (2), 131–137.
Rozina, A.M., Asif, S., Klemeš, J.J., Mubashir, M., Bokhari, A., Sultana, S., Mukhtar, A.,
Emmanuel, O., Okezie, U.M., Iweala, E.J., Ugbogu, E.A., 2021. Pretreatment of red palm
Zafar, M., Bazmi, A.A., Ullah, S., Khan, M.S., 2022a. Conversion of the toxic and
oil extracted from palm fruit (Elaeis guineensis) attenuates carbon tetrachloride
hazardous Zanthoxylum armatum seed oil into methyl ester using green and
induced toxicity in Wistar rats. Phytomedicine plus 1 (4), 100079.
recyclable silver oxide nanoparticles. Fuel 310, 122296.
Emmanuel, O., Elekwa, I., Paul-Joseph, C., Ude, V.C., Egedeuzu, O.G., Ijioma, S.N.,
Rozina, A.M., Elnaggar, A.Y., Teong, L.K., Sultana, S., Zafar, M., Munir, M., Hussein, E.E.,
Amachaghi, V.O., Uche-Ikonne, C., Ugbogu, E.A., 2022a. Protective effects of
Abidin, S.Z.U., 2022b. Sustainable and eco-friendly synthesis of biodiesel from novel
coconut water against the intraperitoneal infused carbon tetrachloride-induced
and non-edible seed oil of Monotheca buxifolia using green nano-catalyst of calcium
toxicity—evaluations of biochemical, haematological and histopathological profiles
oxide. Energy Conversion and Management: X 13, 100142.
in rats. Bulletin of the National Research Centre 46 (1), 1–11.

300
Rozina et al. Waste Management Bulletin 2 (2024) 288–301

Rozina, A.M., Zafar, M., Ali, N., Lu, H., 2017a. Biodiesel synthesis from Saussurea Tamjidi, S., Esmaeili, H., Moghadas, B.K., 2021. Performance of functionalized magnetic
heteromalla (D. Don) Hand-Mazz integrating ethanol production using biorefinery nanocatalysts and feedstocks on biodiesel production: a review study. J. Clean. Prod.
approach. Energy 141, 1810–1818. 305, 127200.
Rozina, Asif, S., Ahmad, M., Zafar, M., Ali, N., 2017b. Prospects and potential of fatty Teo, S.H., Islam, A., Chan, E.S., Choong, S.T., Alharthi, N.H., Taufiq-Yap, Y.H., Awual, M.
acid methyl esters of some non-edible seed oils for use as biodiesel in Pakistan. R., 2019. Efficient biodiesel production from Jatropha curcus using CaSO4/Fe2O3-
Renewable and Sustainable Energy Reviews 74, 687–702. SiO2 core-shell magnetic nanoparticles. J. Clean. Prod. 208, 816–826.
Sarkar, R.D., Singh, H.B., Kalita, M.C., 2021. Enhanced lipid accumulation in microalgae Ugbogu, E.A., Akubugwo, E.I., Ude, V.C., Emmanuel, O., Okomba, N.O., Ibe, C.,
through nanoparticle-mediated approach, for biodiesel production: A mini-review. Onyero, O., 2019. Safety evaluation of an aqueous extract of Termitomyces robustus
Heliyon 7 (9). (Agaricomycetes) in Wistar rats. International Journal of Medicinal Mushrooms 21
Sathish, T., Saravanan, R., Rajasimman, M., Ghfar, A.A., Ramkumar, V., 2023. (2).
Nanoparticle assorted biofuels production from biowastes through Ugbogu, O.C., Emmanuel, O., Agi, G.O., Uche, M.E., Nnanna, R.O., Ugbogu, E.A., 2021.
transesterification. Fuel 331, 125875. A review on the traditional uses, phytochemistry, and pharmacological activities of
Sharma, G.K., Harel, P.G., James, N.R., 2023. Flexible N-doped carbon nanofiber clove basil (Ocimum gratissimum L.). Heliyon 7, e08404.
containing Nb2O5 nanoparticle and its polydimethylsiloxane composite for Ugbogu, E.A., Okoro, H., Emmanuel, O., Ugbogu, O.C., Ekweogu, C.N., Uche, M., Dike, E.
electromagnetic interference shielding. Carbon 214, 118367. D., Ijioma, S.N., 2024. Phytochemical characterization, anti-diarrhoeal, analgesic,
Sheldon, R.A., 2020. Biocatalysis and biomass conversion: Enabling a circular economy. anti-inflammatory activities and toxicity profile of Ananas comosus (L.) Merr
Phil. Trans. R. Soc. A 378 (2176), 20190274. (pineapple) leaf in albino rats. J. Ethnopharmacol. 319, 117224.
Tahir, M.H., Çakman, G., Goldfarb, J.L., Topcu, Y., Naqvi, S.R., Ceylan, S., 2019. Vignesh, N.S., Vimali, E., Sangeetha, R., Arumugam, M., Ashokkumar, B.,
Demonstrating the suitability of canola residue biomass to biofuel conversion via Ganeshmoorthy, I., Varalakshmi, P., 2020. Sustainable biofuel from microalgae:
pyrolysis through reaction kinetics, thermodynamics and evolved gas analyses. application of lignocellulosic wastes and bio-iron nanoparticle for biodiesel
Bioresour. Technol. 279, 67–73. production. Fuel 278, 118326.
Talavari, R., Hosseini, S., Moradi, G.R., 2021. Low-cost biodiesel production using waste Yatish, K.V., Lalithamba, H.S., Suresh, R., Latha, H.K.E., 2020. Ochrocarpus longifolius
oil and catalyst. Waste Manag. Res. 39 (2), 250–259. assisted green synthesis of CaTiO3 nanoparticle for biodiesel production and its
kinetic study. Renew. Energy 147, 310–321.

301